EnvironmEntaL - Waters Corporation · 2010. 10. 28. · Detection: mix M-531M and M-531-IS each...

EnvironmEntaL C h r o m a t o g r a p h y M e t h o d s G u i d e

Waters is Your Partner[for Environmental testing]

nvironmental quality issues are complex, challenging, and ever expanding. Across the globe, regulatory agencies are increasing the amount of environmental testing required to

ensure public safety. Understanding the complex nature of this type of analysis, Waters Corporation is committed to working with its worldwide partners to keep the environment safe.

As demonstrated in this Environmental Chromatography Methods Guide, our solutions have been adopted by regulatory bodies around the globe. With a comprehensive portfolio of products, Waters strives to provide efficient, cost-effective, and compliant solutions for scientists in academia, government, and private testing laboratories.

E

Table of ConTenTs

SubjectEPA Method

Number Title Page

Perchlorates 331.0Determination of Perchlorates in Drinking Water by Liquid Chromatography Electrospray Ionization Mass Spectrometry

6

Carbamates 531.2Measurement of n-Methylcarbamoyloxime and n-Methylcarbamates in Water by Direct Aqueous Injection HPLC with Postcolumn Derivatization

7

Phenylurea Compounds 532.0Determination of Phenylurea Compounds in Drinking Water by Solid Phase Extraction and High Performance Liquid Chromatography with UV Detection

9

Chloroacetanilide and Acetamide Herbicide Degradates

535.0Measurement of Chloracetanilide and Other Acetamide Herbicide Degradates in Drinking Water by Solid Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)

11

Glyphosate 547.0Determination of Glyphosate in Drinking Water by Direct-Aqueous Injection HPLC, Post Column Derivatization and Fluorescence Detection

13

Polycyclic Aromatic Hydrocarbons (PAHs)

550.1Determination of Polynuclear Aromatic Hydrocarbons in Drinking Water by Liquid-Solid Extraction and HPLC with Coupled Ultraviolet and Fluorescence Detection

15

Aldehydes and Ketones as DNPH Derivatives

554.0Determination of Carbonyl Compounds in Drinking Water by Dinitrophenylhydrazine Derivatization and High Performance Liquid Chromatography

17


610.0 Determination of Polynuclear Aromatic Hydrocarbons in Municipal and Industrial Wastewater 18

Pharmaceuticals and Personal Care Products

1694.0 Pharmaceuticals and Personal Care Products in Water, Soil, Sediment and Biosolids 20

Perchlorates 6850.0Determination of Perchlorate in Water, Soils and Solid Wastes using High Performance Liquid Chromatography/Electrospray Ionization/Mass Spectrometry (HPLC/ESI/MS)

29


8310.0 Determination of Polynuclear Aromatic Hydrocarbons in Ground Water and Wastes 30

Explosives 8330.0Determination of Nitroaromatics and Nitramines by High Performance Liquid Chromatography (HPLC)

32

Formaldehyde TO11Determination of Formaldehyde in Ambient Air using Adsorbant Cartridge followed by High Performance Liquid Chromatography

34

Emerging Contaminants and Alternate Methods

Chlorinated Acids 555.0 ACQUITY UPLC System with Photodiode Array (PDA) Detector 35

Perfluorinated Compounds (PFC/PFOS/PFOA)

n/a Emerging Contaminant of Concern 37

Perfluorinated Compounds n/a Advancing Perfluorinated Compound Analysis Using Simultaneious Matrix Monitoring 39

Endocrine Disruptors n/a Emerging Contaminant of Concern 41

Endocrine Disruptors n/aAdvancing Disrupting Compound Analysis Through Integrated Technology and Workflow Solutions

43

Endocrine Disruptors n/aA Sensitive Method for the Determination of Endocrine-Disrupting Compounds in River Water by LC/MS/MS

45

Nerve Agents n/a Determination of Nerve Agent Degradation Products in Drinking Water 47

Priority Pollutants n/aMulti-Residue Analysis of Priority Pollutants in Drinking and Surface Water using Solid-Phase Extraction and GC Tandem Quadrupole MS/MS

48

4

Incorporating hydrophilic-lipophilic balanced water-wettable copolymer, Oasis® products allow

you to achieve robust, selective, and sensitive solid-phase extraction (SPE) methods without

worrying about low recoveries caused by breakthrough, sorbent drying, pH limitations, and

undesirable silanol activity.

CErTifiEd ViAlS

The HPLC Certified vials are the only ones in the market held to tight dimensional requirements,

and guaranteed to be residue free. The LCMS certified vials are MS tested with specifications for

total ion count and presence of clusters in the high mass range.

Sep-Pak® products are recognized worldwide and remain the most referenced SPE products

for GC/MS, HPLC, and LC/MS analysis. Using silica base particles, they offer a versatile and

cost effective solid-phase extraction alternative.

Waters Certified Sep-Pak® SPE cartridges are quality tested to the lowest level of extractables

in the industry. Manufactured using strict performance and cleanliness specifications and

QC-tested for extractables and leachables, Certified Sep-Pak sample preparation products

reduce interference and increase sensitivity by eliminating contaminants introduced by the

cartridge hardware and sorbents.

feaTured produCTs

Environmental Resource Associates is the leading provider of quality assurance, validation,

and certified reference materials to the Environmental industry. ERA products can be used for

wastewater, drinking water, soil, and air analyses.

5

With the state-of-the-art, reversed-phase C18 and C8 bonding and endcapping technology,

SunFire™ columns provide best peak shape for basic compounds, excellent low pH stability, high

efficiency, and greater mass loading capacity.

With an order-of-magnitude improvement in high pH stability and a higher level of chromato-

graphic performance, XBridge™ ethylene bridged hybrid (BEH) columns define the new

benchmark for LC method development with excellent stability over a wide pH range (1-12).

The most technologically advanced LC columns ever created. Designed, tested, and guaran-

teed for use in applications up to 15000 psi (1000 bar), ACQUITY UPLC® columns provide

unsurpassed efficiency, ruggedness, and throughput. Combine faster separations with higher

resolution by harnessing the full potential of sub-2 µm diameter particles.

ENViroNMENTAl SPECiAlTy ColuMNSIn addition to a complete selection of UPLC® and HPLC column chemistries, Waters also

provides columns optimized for the analysis of specific environmental contaminants.

Used worldwide, the Waters PAH and Carbamate columns provide resolution and

sensitivity for cutting edge performance.

The industry’s solution to polar compound retention is designed to retain and separate difficult-

to-analyze polar compounds. Fully LC/MS compatible. Atlantis® columns are available in

three chemistries: T3, HILIC Silica, and dC18.

feaTured produCTs

6

EPA

MET

HOD

331.

0

© 2010 Waters Corporation. Waters, The Science of What’s Possible, Alliance, IC-Pak, Quattro micro, and MassLynx are trademarks of Waters Corporation.

perChloraTes

Perchlorate is both naturally occurring and man-made. In its natural

form, perchlorate is a contaminant in fertilizers. Man-made perchlo-

rate is used in a wide variety of industrial applications including

the production of rubber and paint, in lubricants, and as a primary

ingredient in solid rocket propellant. Perchlorate is highly water

soluble and can migrate into groundwater and surface water, posing

a concern to drinking water supplies. Thirty-five states have detected

perchlorate in drinking water at higher levels than expected. The United

States Environmental Protection Agency (US EPA) has established an

official reference of 0.0007 ppb per day of perchlorate. Maryland,

Massachusetts, and New Mexico have established a one part per

billion (ppb) action limit, while California and Texas have

established 4 ppb limits.

HPlC CoNdiTioNS

Instrument: Alliance® HPLC and conductivity detector

Eluent: 25 mM ammonium bicarbonate, pH = 10 in 50% acetonitrile

Column: IC-Pak™ A/HR, 4.6 x 150 mm, 7 μm @ 30 °C

Injection: 100 μL

Flow Rate: 0.5 mL/min

Data: MassLynx™ software

MS CoNdiTioNS

Instrument: TQ detector or Quattro micro™ API mass spectrometer

Ion Mode: Electrospray negative (ESI -)

Mode: Multiple reaction monitoring (MRM). The MRM transitions,

cone voltages (CV) and collision energies (CE) are listed below.

Compound MrM Transition CV CE

Perchlorate (quantification) 99.1>82.7 40 30

Perchlorate (confirmation) 101.1>84.7 40 30

Internal Standard (Cl18O4-) 107.1>88.7 40 30

Optimized MRM transition parameters for EPA Method 331.0 in ES-.

SAMPlE PrEPArATioN

No sample pretreatment. Add internal standard.

1 ppb perchlorate in HTDS.

0.5 ppb perchlorate detection in three different sample matrices by LC/MS/MS. Analyzed on consecutive days with fresh eluent.

ordEriNg iNforMATioN

related Parts Part Number

IC-Pak Anion HR, 7 μm, 4.6 x 150 mm WAT26770

Perchlorate Standard 186004155

Perchlorate CRM 186004253

LC/MS Certified Vials see catalog

related literature literature Code

Environmental System Solutions 720001601EN

The Determination of Perchlorate in Water Using

LC/MS/MS

720000941EN

The Determination of Perchlorate in Drinking Water

Using Single Quadrupole Mass Spectrometry

720001285EN

www.waters.com/library

0 4 8 12 16 20 24 min

TIC1 ppb ClO4

HTDS defined as:1000 ppb each of HCO3, Cl, and SO4

SO4

Cl

Cations & HCO3

Conductivity ProfileBlank HTDS

50 µ

S FS

Det Limit at 3x S/N < 0.1 ppb

100 µL of0.5 ppb Cl40

Drinking Water

HTDS

Milford

Reagent Waters

SO4Region

Cations &Water Dip

ClRegion

0 4 8 12 16 20 min

Resp

onse

1.2

3 x 1

30

Determination of Perchlorates in Drinking Water by Liquid Chromatography Electrospray Ionization Mass Spectrometry

Continue...

7

EPA

MET

HOD

531.

2

CarbamaTes

Carbamates are used worldwide as commercial pesticides for food

crops. The resulting agricultural runoff can carry them into surface

water, groundwater, and other drinking water resources. The United

States Environmental Protection Agency (US EPA) requires that drink-

ing water and raw surface water be monitored for the presence of

carbamate pesticides and related compounds using an established EPA

Method 531.2. The European Union (EU) regulation regarding drinking

water, provides a general rule for pesticides and metabolites. This regu-

lation limits the maximum admissible concentration (MAC) at 0.1 μg/L

(ppb) for each individual component, with the total concentration not to

exceed 0.5 ppb. Detection of regulated compounds at ever decreasing

levels is a challenge faced by many water testing laboratories. Because

the concentration of these substances in real samples may be in the low

parts per billion (ppb) or μg/L, optimal sensitivity is the ultimate goal.

HPlC CoNdiTioNS

Instument: Alliance® system for carbamate analysis

Eluent: Water/methanol/acetonitrile

Column: Waters Carbamate Analysis column

3.9 x 150 mm @ 30 °C

Injection: 400 μL of standard


Detection: Fluorescence, Ex- 339 nm, Em- 445 nm, Gain- 10

Data: Empower™ software

SAMPlE PrEPArATioN

Oasis® SPE Method for Carbamates

Method for Oasis HLB Cartridge, 6 cc, 200 mg

For LC analysis, exchange to acetonitrile, then adjust to 1 mL.

STANdArd MiX PrEPArATioN

Pipette 25 μL of AccuStandard® mix M-531M and M-531-IS each

into 100 mL of preserved reagent water for a final concentration of

25 parts per billion (ppb) per analyte. Preserved reagent water is

prepared by dissolving 9.35 g of potassium dihydrogen citrate and

0.2 g of sodium thiosulfate (anhydrous) in water and diluting to 1 L.

PREPARE SAMPLE:

Adjust to pH 3

CONDITION:

3 mL MTBE

RINSE:

3 mL methanol

RINSE:

3 mL H2O

LOAD:

Up to 500 mL sample

WASH:

2 mL 5% methanol in H2O

ELUTE:

6 mL 10% methanol/MTBE

Measurement of n-Methylcarbamoyloxime and n-Methylcarbamates in Water by Direct Aqueous Injection HPLC with Postcolumn Derivatization

8

EPA

MET

HOD

531.

2CarbamaTes

© 2010 Waters Corporation. Waters, The Science of What’s Possible, Oasis, Alliance, and Empower are trademarks of Waters Corporation. AccuStandard is a registered trademark of AccuStandard Inc.

EluENT PrEPArATioN

Filter and degas all eluents through a 0.45 µm filter.

A: Water

B: Methanol

C: Acetonitrile

Time flow %A %B %C Curve

Initial 1.5 88.0 12.0 0.0 -

5.30 1.5 88.0 12.0 0.0 1

5.40 1.5 68.0 16.0 16.0 5

14.00 1.5 68.0 16.0 16.0 3

16.10 1.5 50.0 25.0 25.0 7

20.00 1.5 50.0 25.0 25.0 6

22.00 1.5 88.0 12.0 0.0 5

30.00 1.5 88.0 12.0 0.0 1

Eluent gradient.

PoST ColuMN rEAgENT PrEPArATioN

reagent 1: 0.05 N sodium hydroxide

Dissolve 2 g NaOH in water and dilute to 1 L, filter and degas.

reagent 2: PA/2-mercaptoethanol

Dissolve 19.1 g of Borax (Na2B4O7•10H2O) Sodium borate

in 1 L of water. To this, add a solution of 0.1 OPA

(o-phthaldialdehyde) in 10 mL methanol. Swirl to dissolve,

filter, and degas. To this, add 1.0 mL of 2-mercaptoethanol,

ently swirl to dissolve. Protect from light. Post-column

reaction temperature is 80 °C.

Standard chromatogram of 25 ppb for each analyte.

Peak Analyteretention Time

(min)detection limit

(ppb)

1 Aldicarb Sulfoxide 3.77 0.019

2 Aldicarb Sulfone 4.66 0.041

3 Oxamyl 5.17 0.050

4 Methomyl 6.03 0.031

5 3-Hydroxy Carbofuran 9.83 0.022

6 Aldicarb 11.46 0.022

7 Propoxur 14.35 0.038

8 Carbofuran 14.94 0.028

9 Carbaryl 17.37 0.013

10 1-Naphthol 18.99 0.053

11 Methiocarb 22.02 0.022

12 BDMC* 22.56 0.031

* Internal Standard

EPA Method 531.2 target analytes.



Oasis HLB Cartridge, 6 cc, 200 mg WAT106202

Carbamate Analysis Column, 3.9 x 150 mm WAT35577

Carbamate/Carbamoxyloxime Pesticides Standard 186004278

related documents literature Code

Waters Alliance Systems for Carbamate Analysis 720000126EN

Carbamates in Drinking Water 720000609EN

A Fully Automatic Multi-Analyte Quantification

Protocol for Carbamates – A Comparison of LC/MS

and LC/MS/MS

720000672EN

LC/MS of 52 Carbamates: A Fully

Automated Protocol

WA20274


Measurement of n-Methylcarbamoyloxime and n-Methylcarbamates in Water by Direct Aqueous Injection HPLC with Postcolumn Derivatization

20 6 10 14 18 22 min

1

34

5

6

78

9

10

211

12

1500

EU

Continue...

9

EPA

MET

HOD

532.

0

Phenylurea pesticides that were introduced worldwide in the 1950s

are used commercially on a wide range of food crops. Subsequently

determined to possess a significant toxicological risk, the agricultural

runoff of these compounds may be found in drinking water supplies.

The United States Environmental Protection Agency (US EPA)

requires that drinking water and raw surface water be monitored for

the presence of Phenylurea pesticides and related compounds using

EPA Method 532.0. The European Union (EU) regulation regarding

drinking water (EC Directive 98/83/EC), provides a general rule for

pesticides and metabolites. This regulation limits the maximum

admissible concentration (MAC) at 0.1 ppb for each individual

component, with the total concentration not to exceed 0.5 ppb.

HPlC CoNdiTioNS

Instrument: Alliance® HPLC system with 2996 PDA detector

Eluent: A: 25 mM Phosphate, pH 2.4

B: Acetonitrile

Column: SunFire™ C18, 3.5 μm 4.6 x 150 mm @ 30 °C

Injection: 20 μL


Detection: PDA UV @ 245 nm


SAMPlE PrEPArATioN

Oasis® SPE Method for Pheylurea Pesticides

Method for Oasis HLB Cartridge, 6 cc, 200 mg

STANdArd PrEPArATioN

Pipette 100 μL of AccuStandard® mix M-532 and 20 μL mix M-532-SS

into 880 μL 1:1 water/acetonitrile (10 ppm analytes plus surrogates).

EluENT PrEPArATioN

A: 25 mM phosphate

Dissolve 1.7 g of potassium dihydrogen phosphate (KH2PO4) and

850 μL phosphoric acid (H3PO4) in 100 mL water. Dilute to 1 L, then

filter and degas. Verify that the pH is approximately 2.4.

B: Acetonitrile

phenylurea Compounds

PREPARE SAMPLE:

Adjust to pH 3

CONDITION:

3 mL MTBE

RINSE:

3 mL methanol

RINSE:

3 mL H2O

LOAD:

Up to 500 mL sample

WASH:

2 mL 5% methanol in H2O

ELUTE:

5 mL 1:1 ACN/methanol, evaporate

RECONSTITUTE:

1.0 mL initial mobile phase

(500:1 sample enrichment)

Determination of Phenylurea Compounds in Drinking Water by Solid Phase Extraction and High Performance Liquid Chromatography with UV Detection

10

3 5 7 9 11 13 15 min

12

3

4 5

6

7

8

9

10

11

0.45

AU

EPA

MET

HOD

532.

0

© 2010 Waters Corporation. Waters, The Science of What’s Possible, Oasis, Alliance, SunFire, and Empower are trademarks of Waters Corporation. AccuStandard is a registered trademark of AccuStandard Inc.

Time flow %A %B Curve

- 1.5 60 40 -

9.5 1.5 60 40 6

10.0 1.5 50 50 6

14.0 1.5 40 60 6

15.0 1.5 60 40 6

Eluent gradient.

* Surrogate compounds UV @ 245 nm

Standard chromatogram, 10 ppm each analyte.

phenylurea CompoundsDetermination of Phenylurea Compounds in Drinking Water by Solid Phase Extraction and High Performance Liquid Chromatography with UV Detection

Peak Analyte Peak Analyte

1 Tebuthiuron 7 Siduron A

2 Thidiazuron 8 Siduron B

3 Monuron* 9 Linuron

4 Fluometuron 10 Carbazole*

5 Diuron 11 Diflubenzuron

6 Propanil




SunFire C18, 3.5 µm, 4.6 x 150 mm 186002554


Multi-Residue Analysis of Priority Pollutants

in Drinking and Surface Waters Using

Solid-Phase Extraction

720001438EN

Food and Environmental Residue Analysis 720002274EN

Environmental Applications Book 720002123EN


Continue...

11

EPA

MET

HOD

535.

0

Chloroacetanillide and acetamide herbicides are widely used in

the United States for the control of broadleaf and annual weeds

on crops, such as corn and soybeans. These herbicides are thought

to be degraded by microbial action to the oxanilic acid (OA) and

ethanesulfonic acid (ESA) metabolites of the parent compounds.

The OA and ESA metabolites are more water soluble and, therefore,

more mobile than the parent herbicides. Several studies by the United

States Geological Survey (USGS) and others have reported higher

occurrences of the OA and ESA metabolites than the parent herbicides

in both ground and surface water. The United States Environmental

Protection Agency (US EPA) Method 535 was developed for the

determination of OA and ESA metabolites of alachlor, acetochlor,

metochlor, propachlor, flufenacet, and dimetheamide in drinking

water. The European Union (EU) regulation regarding drinking water

(EC Directive 98/83/EC), provides a general rule for pesticides and

metabolites. This regulation limits the maximum admissible concen-

tration (MAC) at 0.1 ppb for each individual component, with the

total concentration not to exceed 0.5 ppb.

lC CoNdiTioNS

Instrument: ACQUITY UPLC® system

Eluent: 5 mM aqeous ammomium acetate/methanol

Column: ACQUITY UPLC BEH C18, 2.1 x 150 mm, 1.7 μm @ 60 °C

Injection: 50 μL


Data: MassLynx™ software

MS CoNdiTioNS

Instrument: TQ detector or Quattro micro™ API mass spectrometer

Ion Mode: Electrospray negative (ESI -)

Mode: Multiple reaction monitoring (MRM). The MRM transitions,

cone voltages (CV) and collision energies (CE) are listed in

in the top right column.

Compound list MrM Transition CV CE

1 Propachlor OA 206.3>134.2 13 11

2 Flufenacet OA 224.3>152.3 13 11

3 Propachlor ESA 256.3>80.0 35 25

4 Flufenacet ESA 274.3>80.0 35 25

5 Dimethenamid OA 270.3>198.3 15 11

6 Dimethenamid ESA 320.3>80.0 40 30

7 Acetachlor OA 264.1>146.2 20 11

8 Alachlor OA 264.1>160.1 20 11

9 Metolachlor OA 278.4>206.3 20 11

10 Alachlor ESA 314.1>80.0 40 25

11 Acetachlor ESA 314.1>80.0 40 25

12 Metolachlor ESA 328.2>80.0 37 25

13 Butachlor ESA 356.2>80.0 35 25

Optimized MRM transition parameters for EPA Method 535 in ESI -.

SAMPlE PrEPArATioN

A 250 mL water sample is extracted using a graphitized carbon SPE

cartridge, dried and made up to 1 mL with 5 mM ammonium acetate.

EluENT PrEPArATioN

A: 5 mM aqueous ammonium acetate

B: Methanol

Time flow %A %B

Initial 0.45 90 10

5.0 0.45 75 25

7.5 0.45 66 34

10.5 0.45 65 35

11.0 0.45 10 90

13.0 0.45 90 10

Eluent gradient.

ChloroaCeTanilide and aCeTamide herbiCide degradaTesMeasurement of Chloracetanilide and Other Acetamide Herbicide Degradates in Drinking Water by

Solid Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)




SunFire C18, 3.5 µm, 4.6 x 150 mm 186002554


Multi-Residue Analysis of Priority Pollutants

in Drinking and Surface Waters Using


720001438EN

Food and Environmental Residue Analysis 720002274EN

Environmental Applications Book 720002123EN


12

EPA

MET

HOD

535.

0

© 2010 Waters Corporation. Waters, The Science of What’s Possible, ACQUITY UPLC, MassLynx, UPLC and Quattro micro are trademarks of Waters Corporation.

UPLC®/MS/MS chromatogram for EPA Method 535 analytes.



ACQUITY UPLC BEH C18, 1.7 µm, 2.1 x 150 mm 186002353

Pesticides Standard 186004280



Acetamide Herbicides and Metabolites

in Drinking Water

oasis24

Analysis of Chloroacetanilide and Acetamide

Herbicide Degradates in Drinking Water

by UPLC/MS/MS

720001999EN


ChloroaCeTanilide and aCeTamide herbiCide degradaTes

0 10 20 30 min

%

0

100

3

4

5

6

7

8

9

10

11

12

13

1

2

100

%

0

4 6 8 12 min10

Measurement of Chloracetanilide and Other Acetamide Herbicide Degradates in Drinking Water by Solid Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)

Continue...

13

EPA

MET

HOD

547.

0

Glyphosate is a non-selective herbicide which is adsorbed through

leaves and was first sold by Monsanto® under the Roundup® trade

name. This is one of the most widely used herbicides, regularly used for

agriculture, horticulture, and silviculture applications. The United States

Environmental Protection Agency (US EPA) requires that drinking water

and raw surface water be monitored for the presence of glyphosate and

related compounds using EPA Method 547.0. The European Union (EU)

regulation (EC Directive 2005/70/EU) provides guidance with regards

to the presence of glyphosate in drinking water supplies.

HPlC CoNdiTioNS

Instrument: Alliance® system for carbamate analysis

Eluent: 0.05% phosphoric acid

Column: Ion Exclusion, 7.8 mm x 150 mm @ 55 °C

Guard: Guard-Pak™ module and inserts

Injection: 200 μL of standard mix

Flow Rate: 1.5 mL / min

Detection: Fluorescence, Ex- 340 nm, Em- 455 nm, Gain- 10

SAMPlE PrEPArATioN

Refer to EPA Method 547 for preparation of field grab samples.

Filter through 0.45 μm Acrodisc® filters is described.

AlTErNATiVE SAMPlE PrEPArATioN

Oasis® MAX SPE Method for Glyphosate and Metabolite

Method for Oasis MAX Cartridge, 6 cc, 150 mg

* Alternate eluent is 4 mL 0.6 M sodium citrate

Use 6 cc, 500 mg Oasis MAX for samples > 50 mL.

STANdArd MiX PrEPArATioN

Pipette 100 μL of AccuStandard® mix (M-547) into 100 mL of

acidified water for a concentration of 100. Prepare acidified water

by adjusting the pH of HPLC grade water to 3.0 by dropwise addition

of hydrochloric acid (HCL). Use EPA Method 547-02 as above for

AMPA (aminomethyl phosphonic acid).

EluENT PrEPArATioN

Dilute 0.5 mL of 85% phosphoric acid (H3PO4) to 1 L, mix well,

filter and degas.

glyphosaTe

PREPARE SAMPLE:

pH 6-8

CONDITION:

2 mL methanol, 4 mL 0.5 M NaOH, 2 mL H2O

RINSE:

4 mL 0.5 M NaOH

RINSE:

2 mL H2O

LOAD:

25 mL sample

WASH:

2 mL H2O

ELUTE:

4 mL 0.5 M HCI in acetonitrile*

EVAPORATE AND RECONSTITUTE:

Adjust to LC analysis

Determination of Glyphosate in Drinking Water by Direct Aqueous Injection HPLC, Post Column Derivatization and Fluorescence Detection

14

EPA

MET

HOD

547.

0

PoST ColuMN rEAgENT PrEPArATioN

reagent 1: Hypochlorite

Dissolve 1.35 g KH2PO4, 11.6 g NaCl, 0.4 g NaOH, and

0.2 mL Clorox® Bleach (plain) in water and dilute to 1 L,

filter and degas.reagent 2: oPA

Dissolve 0.8 g of OPA (o-phthdialdehyde) in 10 mL of

methanol, add this to an aqueous solution of 19.1 g of

Borax Na2B4O7•10H2O. Make to a final volume of 1 L,

filter and degas. To this, add 2 mL of 2-mercaptoethanol,

swirl gently to mix. Protect from light.

Note: Post-column flow rate for both reagents is 0.5 mL/min, post column reaction temperature is 38 °C. Insert second reaction coil in line before the fluorescence detector.

Standard chromatogram, 100 ppb each analyte.



IC-Pak™ Ion-Exclusion Column, 7.8 x 150 mm WAT010295

Guard-Pak Holder WAT88141

Semivolatiles #2 Herbicide Standard 186004271

Oasis MAX Cartridge, 6 cc, 150 mg 186000370

Oasis MAX Cartridge, 6 cc, 500 mg 186000865



Glyphosate and AMPA in Drinking Water WA31764.94

An LC/MS/MS Multi-Analyte Detection Method for

Deleterious Organics in Drinking Water

720001090EN


glyphosaTe

2 6 10 14 18 22 min

1

2

1400

EU

Determination of Glyphosate in Drinking Water by Direct Aqueous Injection HPLC, Post Column Derivatization and Fluorescence Detection

© 2010 Waters Corporation. Waters, The Science of What’s Possible, Alliance, Guard-Pak, IC-Pak and Oasis are trademarks of Waters Corporation. AccuStandard is a registered trademark of AccuStandard Inc. Acrodisc is a registered trademark of Pall Corporation. Monsanto and Roundup are registered trademarks of The Monsanto Company. Clorox is a registered trademark of The Clorox Company.

Peak Analyte

1 Glyphosate

2 AMPA

Continue...

15

polyCyCliC aromaTiC hydroCarbons (pahs)

Polycyclic aromatic hydrocarbons (PAHs) are one of the most widespread

organic pollutants. PAHs are made up of fused aromatic rings and are

formed during the combustion of carbon based fuels (wood, coal, diesel),

as well as being present in crude oil. The United States Environmental

Protection Agency (US EPA) has classified seven PAH compounds as

being potentially carcinogenic including benz[a]anthracene, benzo[a]

pyrene, benzo[b]fluoranthene, benzo[k]fluoranthene, chrysene,

dibenz[a,h]anthracene, and indeno[1,2,3-cd]pyrene.

HPlC CoNdiTioNS

Instrument: Alliance® HPLC system with PDA and

fluorescence detectors

Eluent: Water/acetonitrile (see Detection)

Column: Waters PAH 4.6 x 250 mm (part no. 186001265) @ 30 °C

Injection: 20 μL of Supelco® Standard EPA 610 (#48743) diluted

1:50 in 40:60 water/acetonitrile


Detection: UV @ 254 nm and fluorescence using timed

programmed wavelengths


SAMPlE PrEPArATioN

Extract with C18 cartridge, elute with MeCl2

EluENT PrEPArATioN

Filter and degas through a 0.45 µm filter.

A: Water

B: Acetonitrile


Initial 1.2 40 60 -

12.0 1.2 0 100 9

23.0 1.2 40 60 11

Eluent gradient.

AnalyteuV Max (nm)

EX (nm)

EM (nm)

detection limit (ppb)1

1 Naphthalene 220 277 330 0.14

2 Acenaphthylene 229 NA NA NA

3 Acenaphthene 227 270 323 0.01

4 Fluorene 261 265 310 0.03

5 Phenanthrene 251 252 365 0.02

6 Anthracene 252 250 402 0.01

7 Fluoranthene 236 284 467 0.02

8 Pyrene 240 332 378 0.01

9 Benzo(a)anthracene 287 284 390 0.01

10 Chrysene 267 270 367 0.04

11 Benzo(b)fluoranthene 256 298 436 0.09

12 Benzo(k)fluoranthene 307 303 432 0.01

13 Benzo(a)pyrene2 296 280 410 0.03

14 Dibenzo(a,h)anthracene 297 294 398 0.01

15 Benzo(g,h,I)perylene 299 290 420 0.03

16 Indeno(1,2,3-cd )pyrene 250 305 480 0.49

1 Fluorescence mode used for detection limit determination, no pre-concentration. Seven replicates per 40 CFR pt. 136 App. B.

2 Regulated compound; action level 0.17 ppb.

PAH target analytes.

Standard chromatogram, UV @ 254 nm, 1-20 ppm PAH analytes.

6 10 14 18 22 min

0.05

AU

1

2

3

45

6

7

8

9

10

11

1213

1415 16

Determination of Polycyclic Aromatic Hydrocarbons in Drinking Water by Liquid-Solid Extraction and High Performance Liquid Chromatography with Ultraviolet Detection

EPA

MET

HOD

550.

1

16

6 10 14 18 22 min

1

3

4

5

6

7

8

9

10 11

1213 14

1516

8000

EU


Standard chromatogram, fluorescence/programmed wavelengths, 1-20 ppm

PAH analytes.



PAH Column, 4.6 x 250 mm 186001265

Semivolatiles #1 Standard 186004270

related documentst literature Code

The Determination of Biodegradation Products

of PAH Using LC/MS/MS

WA20747

PAHs in Drinking Water – Oasis® Solution WA31764.127

Waters PAH Columns Improve Analysis

of PAH Compounds

720000382EN


© 2010 Waters Corporation. Waters, The Science of What’s Possible, Alliance, Oasis, and Empower are trademarks of Waters Corporation. Supelco is a registered trademark of Sigma-Aldrich Co.

Determination of Polycyclic Aromatic Hydrocarbons in Drinking Water by Liquid-Solid Extraction and High Performance Liquid Chromatography with Ultraviolet Detection

aldehydes and KeTones as dnph derivaTivesEP

A M

ETHO

D 55

0.1

17

© 2010 Waters Corporation. Waters, The Science of What’s Possible, Alliance, XBridge, Empower, and Oasis are trademarks of Waters Corporation. AccuStandard is a registered trademark of AccuStandard Inc.

Large quantities of carbonyl compounds are used worldwide,

primarily in the chemical and plastics industries. Demonstrated to

be potentially carcinogenic, these compounds have been found in

industrial waste where they can to leach into groundwater supplies

and contaminate drinking water.

HPlC CoNdiTioNS

Instrument: Alliance® HPLC system with UV detection

Eluent: Water/tetrahydrofuran/acetonitrile

Column: XBridge™ Phenyl, 3.5 μm, 4.6 x 150 mm @ 35 °C

Injection: 20 μL each of AccuStandard® mix (M- 8315-R1- DNPH and

M- 8315-R2- DNPH) diluted 1:5 in 40:60 water/acetonitrile


Detection: UV @ 360 nm


SAMPlE PrEPArATioN

DNPH reagent added to 100 mL sample, extract with Oasis® HLB or

use methylene chloride extraction option.

EluENT PrEPArATioN

Filter and degas through a 0.45 μm filter.

A: 90% water, 10% tetrahydrofuran (THF).

Mix 900 mL water and 100 mL stabilized THF.

B: Acetonitrile


Initial 1.5 70 30 -

20.0 1.5 36 64 6

22.0 1.5 36 64 6

22.1 1.5 70 30 6

Eluent gradient for EPA Methods 554.0 and 8315 Option 1.


Initial 1.5 70 30 -

16.0 1.5 53 47 6

21.0 1.5 53 47 6

21.1 1.5 70 30 6

Eluent gradient for EPA Methods TO11 and 8315 Option 2.

EPA Method 554.0 and 8315-01 analytes, 20 parts per million (ppm) as DNPH analytes.



XBridge Phenyl, 3.5 µm, 4.6 x 150 mm 186003335

Oasis HLB, 3 cc, 60 mg WAT094226


Analysis of DNPH Derivatives Using XBridge Phenyl WA60186

Fast Analysis of Aldehydes and Ketones using UPLC 720001860EN


aldehydes and KeTones as dnph derivaTives

1

12111098

76

5

43

2

0.20

AU

4 8 12 16 20 min

Determination of Carbonyl Compounds in Drinking Water by Dinirtophenyldydrazine Derivatization and High Performance Liquid Chromatography


1 Formaldehyde 7 Pentanal

2 Acetaldehyde 8 Hexanal

3 Propanal 9 Heptanal

4 Crotonaldehyde 10 Octanal

5 Butanal 11 Nonanal

6 Cyclohexanone Decanal

EPA

MET

HOD

554.

0

18

Polycyclic aromatic hydrocarbons (PAHs) are one of the most widespread

organic pollutants. PAHs are made up of fused aromatic rings and are

formed during the combustion of carbon based fuels (wood, coal, diesel),

as well as being present in crude oil. The United States Environmental

Protection Agency (US EPA) has classified seven PAH compounds as

being potentially carcinogenic including benz[a]anthracene, benzo[a]

pyrene, benzo[b]fluoranthene, benzo[k]fluoranthene, chrysene,

dibenz[a,h]anthracene, and indeno[1,2,3-cd]pyrene.

HPlC CoNdiTioNS

Instrument: Alliance® HPLC system with PDA and fluorescence detectors

Eluent: Water/acetonitrile

Column: Waters PAH 4.6 x 250 mm @ 30 °C

Injection: 20 μL of Supelco® Standard EPA 610 (#48743)

diluted 1:50 in 40:60 water/acetonitrile





SAMPlE PrEPArATioN

Liquid/liquid extraction with MeCl2

EluENT PrEPArATioN


A: Water

B: Acetonitrile


Initial 1.2 40 60 -

12.0 1.2 0 100 9

23.0 1.2 40 60 11

Eluent gradient.


Standard chromatogram, fluorescence/programmed wavelengths, 1-20 ppm PAH analytes.


6 10 14 18 22 min

0.05

AU

1

2

3

45

6

7

8

9

10

11

1213

1415 16

6 10 14 18 22 min

1

3

4

5

6

7

8

9

1011

1213 14

1516

8000

EU

Determination of Polycyclic Aromatic Hydrocarbons in Municipal and Industrial Wastewater

EPA

MET

HOD

610.

0

19

EPA

MET

HOD

610.

0


© 2010 Waters Corporation. Waters, The Science of What’s Possible, Alliance, and Empower are trademarks of Waters Corporation. Supelco is a registered trademark of Sigma-Aldrich Co.

AnalyteuV max

(nm)EX

(nm)EM

(nm)detection

limit (ppb)1

1 Naphthalene 220 277 330 0.14


3 Acenaphthene 227 270 323 0.01

4 Fluorene 261 265 310 0.03

5 Phenanthrene 251 252 365 0.02

6 Anthracene 252 250 402 0.01

7 Fluoranthene 236 284 467 0.02

8 Pyrene 240 332 378 0.01


10 Chrysene 267 270 367 0.04



13 Benzo(a)pyrene2 296 280 410 0.03



16 Indeno(1,2,3-cd)pyrene 250 305 480 0.491 Fluorescence mode used for detection limit determination, no pre-concentration. Seven replicates per 40 CFR pt. 136 App. B.

2 Regulated compound; action level 0.17 ppb.




PAH Column, 4.6 x 250 mm 186001265



The Determination of Biodegradation Products

of PAH Using LC/MS/MS

WA20747

PAHs in Drinking Water – Oasis Solution WA31764.127

Waters PAH Columns Improve Analysis of PAH

Compounds

720000382EN


Determination of Polycyclic Aromatic Hydrocarbons in Municipal and Industrial Wastewater

20

Many hundreds of active compounds are used in both human and veterinary drug formulations. Due to the many different applications related

to pharmaceuticals, their residues can reach the environment in multiple ways including excretion and manufacturing discharge. These

compounds are not completely eliminated via sewage treatment plants, thus, they can reach surface and groundwater supplies. Recently,

there has been increased interest in monitoring for the presence of pharmaceuticals in drinking water supplies and examining their long term

effects on human health.

HPlC CoNdiTioNS

Instrument: Waters 2690 HPLC or Waters 2795 HPLC, Quattro Ultima® MS/MS

Column: XTerra® C18, 3.5 μm, 2.1 x 100 mm

Ionization: ESI+

Acquisition: MRM mode, unit resolution

Injection Volume: 15 μL

lC gradient Program lC flow rate (ml/min)

gradientgeneral lC Conditions

Time (min) flow Mixture1 Column Temperature 40 °C

0.095% Solvent A

5% Solvent B0.150 1 Flow Rate 0.15-0.30 mL/min

4.095% Solvent A

5% Solvent B0.250 6 Max Pressure 345 Bar

22.512% Solvent A

88% Solvent B0.300 6

Autosampler Tray

Temperature4 °C

23.0 100% Solvent B 0.300 6 MS Conditions

26.0 100% Solvent B 0.300 6 Source Temperature 140 °C

26.595% Solvent A

5% Solvent B0.150 6 Desolvation Temperature 350 °C

33.095% Solvent A

5% Solvent B0.150 6

Cone/Desolvation

Gas Rate80 L/hr /400 L/hr

1 Solvent A = 0.3% Formic Acid and 0.1% Ammonium Formate in HPLC water

Solvent B = 1:1 Acetonitrile:Methanol

Group 1 – Acidic extraction, positive electrospray ionization (ESI+) instrument conditions.

EPA

MET

HOD

1694

pharmaCeuTiCals and personal Care produCTsPharmaceuticals and Personal Care Products in Water, Soil, Sediment and Biosolids by HPLC/MS/MS

21

Continue...

EPA

MET

HOD

1694


AnalyterT

(min)Parent-daughter

M/ZSQuantitation

reference

detection limits and Minimum levels

Water (ng/l) other (μg/kg) Extract (ng/Φl)

Mdl Ml Mdl Ml Mdl Ml

group 1 Analytes Extracted under Acidic Conditions and Analyzed using Positive Electrospray ionization (ESi+)

Native Compounds

Sulfanilamide 2.5 190.0 - 155.8 13C6 -Sulfamethazine 8.9 50 48 200 2.2 12.5

Cotinine 2.8 177.0 – 98.0 Cotinine-d3 3.4 5 1.1 5 0.9 1.25

Acetaminophen 4.6 152.2 – 110.013C2-15N-

Acetaminophen27 200 35 200 6.7 50

Sulfadiazine 6.0 251.2 – 156.1 13C6-Sulfamethazine 0.4 5 2.7 10 0.1 1.25

1,7-Dimethylxanthine 6.9 181.2 – 124.0 13C3-Caffeine 120 500 270 1000 30 125

Sulfathiazole 7.7 256.3 – 156.0 13C6-Sulfamethoxazole 0.5 5 1.9 50 0.1 1.25

Codeine 8.3 300.0 – 152.0 13C3-Trimethoprim 1.5 10 3.4 10 0.4 2.5

Sulfamerazine 8.7 265.0 – 156.0 13C6-Sulfamethazine 0.3 2 1.4 5 0.1 0.5

Lincomycin 9.3 407.5 – 126.0 13C3-Trimethoprim 0.8 10 4.7 10 0.2 2.5

Caffeine 9.3 195.0 – 138.0 13C3-Caffeine 15 50 5.4 50 3.6 12.5

Sulfamethizole 10.0 271.0 – 156.0 13C6-Sulfamethoxazole 0.4 2 0.88 5 0.1 0.5

Trimethoprim 10.0 291.0 – 230.0 13C3-Trimethoprim 1.1 5 3.3 10 0.3 1.25

Thiabendazole 10.0 202.1 – 175.1 Thiabendazole-d6 0.7 5 2.1 10 0.2 1.25

Sulfamethazine 10.1 279.0 – 156.0 13C6-Sulfamethazine 0.6 2 0.83 5 0.2 0.5

Cefotaxime 10.2 456.4 – 396.1 13C3-Trimethoprim 10 20 18 50 2.5 5

Carbadox 10.5 263.2 – 231.2 13C3-Trimethoprim 2.3 5 2.1 10 0.6 1.25

Ormetoprim 10.5 275.3 – 259.1 13C3-Trimethoprim 0.3 2 0.50 2 0.1 0.5

Norfloxacin 10.7 320.0 – 302.0 13C3 15N-Ciprofloxacin 28 50 15 50 7.0 12.5

Sulfachloropyridazine 10.8 285.0 – 156.0 13C6-Sulfamethazine 1.2 5 1.9 5 0.3 1.25

Ofloxacin 10.8 362.2 – 318.0 13C3 15N-Ciprofloxacin 1.8 5 3.4 10 0.4 1.25

Ciprofloxacin 10.9 332.2 – 314.2 13C3 15N-Ciprofloxacin 5.1 20 8.1 20 1.3 5

Clinafloxacin 12.2 366.3 – 348.0 13C3 15N-Ciprofloxacin 6.9 20 14 50 1.7 5

Digoxigenin 12.6 391.2 – 355.2 13C3-Trimethoprim 5.7 20 9.4 20 1.4 5

Oxolinic acid 13.1 261.8 – 243.8 13C3-Trimethoprim 0.6 2 0.62 2 0.2 0.5

Sulfadimethoxine 13.2 311.0 – 156.0 13C6-Sulfamethoxazole 0.1 1 0.55 2 0.03 0.25

Diphenhydramine 14.5 256.8 – 168.1 13C3-Trimethoprim 0.4 2 0.66 2 0.1 0.5

Penicillin G 14.6 367.5 – 160.2 13C3-Trimethoprim 2.4 10 13 50 0.6 2.5

Azithromycin 14.8 749.9 – 591.6 13C3-Trimethoprim 1.3 5 1.6 5 0.3 1.25

Flumeqine 15.2 262.0 – 173.7 13C3-Trimethoprim 2.7 5 1.4 5 0.7 1.25

Ampicillin 15.3 350.3 – 160.2 13C3-Trimethoprim - 5 - 5 - 1.25

Diltiazem 15.3 415.5 – 178.0 13C3-Trimethoprim 0.6 2 0.30 2 0.2 0.25

Carbamazepine 15.3 237.4 – 194.2 13C3-Trimethoprim 1.4 5 1.6 5 0.4 1.25

Penicillin V 15.4 383.4 – 160.2 13C3-Trimethoprim 4.4 20 19 50 1.1 5

Erythromycin 15.9 734.4 – 158.0 13C2-Erythromycin - 1 - 2 - 0.25

Tylosin 16.3 916.0 – 772.013C2-Erythromycin

anhydrate13 50 8.1 50 3.2 5

Oxacillin 16.4 434.3 – 160.1 13C3-Trimethoprim 3.3 10 9.4 20 0.8 2.5

Dehydronifedipine 16.5 345.5 – 284.1 13C3-Trimethoprim 0.6 2 0.41 2 0.2 0.5

22

AnalyterT


M/ZSQuantitation

reference


Water (ng/l) other (μg/kg) Extract (ng/Φl)



Native Compounds

Clarithromycin 17.5 748.9 – 158.213C2-Erythromycin

anhydrate1.0 5 1.2 5 0.3 1.25

labeled compounds spiked into each sample

Cotinine-d3 2.8 180.0 – 79.9 13C3-Atrazine13C2-15N-

Acetaminophen4.5 155.2 – 111.0 13C3-Atrazine

13C3 Caffeine 9.3 198.0 – 140.0 13C3-Atrazine

Thiabendazole-d6 9.8 208.1 – 180.1 13C3-Atrazine13C3-Trimethoprim 10.0 294.0 – 233.0 13C3-Atrazine13C6 Sulfamethazine 10.1 285.1 – 162.0 13C3-Atrazine13C3

15N-Ciprofloxacin 10.9 336.1 – 318.0 13C3-Atrazine13C6-Sulfamethoxazole 11.2 260.0 – 162.0 13C3-Atrazine13C2-Erythromycin 15.9 736.4 – 160.0 13C3-Atrazine

Fluoxetine-d5 16.8 315.3 – 153.0 13C3-Atrazine13C2-Erythromycin

anhydrate17.7 718.4 – 160.0 13C3-Atrazine

injection internal standard

13C3 Atrazine 15.9219.5 – 176.9

(134.0)External standard

Group 1 – Acidic extraction, positive electrospray ionization (ESI+) compound retention times (RTs), parent-daughter transitions, quantitation references, method detection limits, and minimum levels of quantitation.

EPA

MET

HOD

1694

pharmaCeuTiCals and personal Care produCTs Pharmaceuticals and Personal Care Products in Water, Soil, Sediment and Biosolids by HPLC/MS/MS

Continue...

23

EPA

MET

HOD

1694


HPlC CoNdiTioNS

Instrument: Waters 2690 HPLC or 2795 HPLC, Quattro Ultima MS/MS

Column: XTerra C18, 3.5 μm 2.1 x 100 mm

Ionization: ESI+


Injection: 5 μL




0.010% Solvent A

90% Solvent B0.20 1 Flow Rate 0.20-0.23 mL/min

1.010% Solvent A


18.040% Solvent A

60% Solvent B0.23 6

Autosampler Tray

Temperature4 °C

20.090% Solvent A

10% Solvent B0.23 6 MS Conditions

24.090% Solvent A

10% Solvent B0.23 6 Source Temperature 120 °C

24.310% Solvent A


2810% Solvent A

90% Solvent B0.20 6 Cone / Desolvation Gas Rate 70 L/hr /450 L/hr

1 Solvent A = 1:1 acetonitrile:methanol, with 5 mM Oxalic Acid Solvent B = HPLC H2O, with 5 mM Oxalic Acid.

Group 2 – Acidic extraction positive electrospray ionization (ESI+) instrument conditions.

24

AnalyterT


M/ZSQuantitation

reference


Water (ng/l) other (ng/g) Extract (ng/μl)



Native Compounds

Minocycline 5.1 458.0 – 441.0 Thiabendazole-d6 51 200 - 200 13 50

Epitetracycline 8.1 445.2 – 410.2 Thiabendazole-d6 3.6 20 8.6 20 0.9 5

Epioxytetracycline (EOTC) 8.6 461.2 – 426.2 Thiabendazole-d6 4.1 20 18 50 1.0 5

Oxytetracycline (OTC) 9.4 461.2 – 426.2 Thiabendazole-d6 2.1 20 2.2 20 0.5 5

Tetracycline (TC) 9.9 445.2 – 410.2 Thiabendazole-d6 1.9 20 2.8 20 0.5 5

Demeclocycline 11.7 465.0 – 430.0 Thiabendazole-d6 6.6 50 7.9 50 1.7 12.5

Isochlortetracycline (ICTC)1 11.9 479.0 – 462.2 Thiabendazole-d6 1.7 20 3.5 20 0.4 5

Epichlortetracycline (ECTC)1 12.0 479.0 – 444.0 Thiabendazole-d6 7.7 50 26 100 1.9 12.5

Chlortetracycline (CTC) 14.1 479.0 – 444.0 Thiabendazole-d6 1.2 20 2.3 20 0.3 5

Doxycycline 16.7 445.2 – 428.2 Thiabendazole-d6 2.8 20 2.3 20 0.7 5

Epianhydrotetracycline (EATC) 17.0 426.8 – 409.8 Thiabendazole-d6 7.7 50 14 50 1.9 12.5

Anhydrotetracycline (ATC) 18.8 426.8 – 409.8 Thiabendazole-d6 4.6 50 7.1 50 1.2 12.5

Epianhydrochlortetracycline

(EACTC)20.7 461.2 – 444.0 Thiabendazole-d6 28 200 23 200 7.0 50

Anhdrochlortetracycline

(ACTC)22.1 461.2 – 444.0 Thiabendazole-d6 5.2 50 11 50 1.3 12.5

labeled compound spiked into each sample

Thiabendazole-d6 7.0 208.1 – 180.1 13C3-Atrazine

injection internal standard

13C3-Atrazine 10.5219.5 – 176.9

(134.0)External standard

1 Isochlortetracycline (ICTC) is reported as the sum ICTC + ECTC due to a common transition ion.

Group 2 – Acidic extraction positive electrospray ionization (ESI+) compound retention times (RTs), parent-daughter transitions, quantitation references, method detection limits, and minimum levels of quantitation.

EPA

MET

HOD

1694


Continue...

25

EPA

MET

HOD

1694


HPlC CoNdiTioNS


Column: XTerra C18, 3.5 μm, 2.1 x 100 mm

Ionization: ESI-


Injection: 5 μL




0.060% Solvent A

40% Solvent B0.2 1 Flow Rate 0.200 mL/min

0.560% Solvent A


7.0 100% Solvent B 0.2 6Autosampler Tray

Temperature4 ºC

12.5 100% Solvent B 0.2 6 MS Conditions

12.760% Solvent A


16.060% Solvent A


Cone/Desolvation Gas Rate 50L/hr /300 L/hr1 Solvent A = 0.1% Ammonium Acetate and 0.1% Acetic Acid in HPLC water Solvent B = 1:1 MethanolAcetonitrile

Group 3 – Acidic extraction negative electrospray ionization (ESI-) instrument conditions.

26

AnalyterT

(min)

Parent-daughter

M/ZS

Quantitation reference


Water (ng/l) other (Φg/g) Extract (ng/Φl)


group 3 Analytes Extracted under Acidic Conditions and Analyzed using Negative Electrospray ionization (ESi-)

Native Compounds

Naproxen 6.7 228.9 – 168.6 13C-Naproxen-d3 3.9 10 6.1 20 1.0 2.5

Warfarin 7.1 307.0 – 117.0 Warfarin-d5 0.9 5 1.6 5 0.2 1.25

Ibuprofen 8.4 205.1 – 161.1 13C3-Ibuprofen 6.0 50 11 50 1.5 12.5

Gemfibrozil 9.5 249.0 – 121.0 Gemfibrozil-d6 0.8 5 1.2 5 0.2 1.25

Triclocarban 9.6 312.9 – 159.7 13C6-Triclocarban 2.1 10 2.7 10 0.5 2.5

Triclosan 9.7 286.8 – 35.0 13C12-Triclosan 92 200 56 200 23 50

labeled compounds spiked into samples13C-Naproxen-d3 6.6 232.9 – 168.6 13C6-TCPAA

Warfarin-d5 7.0 312.0 – 161.0 13C6-TCPAA13C3-Ibuprofen 8.5 208.2 – 163.1 13C6-TCPAA

Gemfibrozil-d6 9.5 255.0 – 121.0 13C6-TCPAA13C6-Triclocarban 9.6 318.9 – 159.7 13C6-TCPAA13C12-Triclosan 9.7 298.8 – 35.0 13C6-TCPAA

injection internal Standard13C6-TCPAA 4.9 258.8 – 200.7 External standard

Group 3 – Acidic extraction negative electrospray ionization (ESI-) compound retention times (RTs), parent-daughter transitions, quantitation references, method detection limits, and minimum levels of quantitation.

EPA

MET

HOD

1694


Continue...

27

EPA

MET

HOD

1694


HPlC CoNdiTioNS


Column: Atlantis® HILIC, 3.0 μm, 2.1 x 100 mm

Ionization: ESI+


Purge Solvent: 100% CH3CN (changed from H2O)

Injection: 2.0 μL




0.02% Solvent A

8% Solvent B0.25 1 Flow Rate 0.25 mL/min

5.030% Solvent A


12.030% Solvent A

70% Solvent B0.25 6

Autosampler Tray

Temperature4 °C

12.52% Solvent A

98% Solvent B0.25 6 MS Conditions

16.02% Solvent A


Desolvation Temperature 350 °C

Cone/Desolvation Gas Rate 70L/hr /400 L/hr1 Solvent A = 0.1% Acetic Acid/Ammonium Acetate Buffer Solvent B = Acetonitrile

Group 4 – Basic extraction positive electrospray ionization (ESI+) instrument conditions.

28

AnalyterT

(min)

Parent-daughter

M/ZS

Quantitation reference


Water (ng/l) other (ng/g) Extract (ng/Φl)


group 4 Analytes Extracted under Acidic Conditions and Analyzed using Positive Electrospray ionization ESi+

Native Compounds

Cimetidine 6.9 253.1 – 159.0 Albuterol-d3 0.6 2 0.78 2 0.2 0.5

Albuterol 9.4 240.0 – 148.0 Albuterol-d3 0.9 2 0.39 2 0.2 0.5

Ranitidine 10.3 315.0 – 175.9 Albuterol-d3 0.7 2 1.1 2 0.2 0.5

Metformin 11.0 131.1 – 60.1 Metformin-d6 23 100 38 100 5.8 25

labeled compounds spiked into samples

Albuterol-d3 9.4 243.0 – 151.0 Cotinine-d3

Metformin-d6 11.0 285.1 – 163.0 Cotinine-d3

injection internal Standard

Cotinine-d3 5.9 180.0 – 79.9 External standard

13C3-Atrazine 2.0219.5 – 176.9

(134.0)External Standard

Group 4 – Basic extraction positive electrospray ionization (ESI+) compound retention times (RTs), parent-daughter transitions, quantitation references, method detection limits, and minimum levels of quantitation.

pharmaCeuTiCals and personal Care produCTs

© 2010 Waters Corporation. Waters, The Science of What’s Possible, Quattro Ultima, XTerra, Atlantis, and Oasis are trademarks of Waters Corporation.

Pharmaceuticals and Personal Care Products in Water, Soil, Sediment and Biosolids by HPLC/MS/MS



XTerra MS C18, 3.5 μm, 2.1 x 100 mm 186000404

Atlantis HILIC, 3.0 μm, 2.1 x 100 mm 186002013

Oasis® HLB Extraction Cartridge, 20 cc, 1g, LP 186000117

EPA Method 1694 Analysis Kit 176001634



Total Solutions for Environmental Applications 720002163EN

LC/MS Determination of Pharmaceutical Residues

in Environmental Samples

720000421EN


EPA

MET

HOD

1694

29

EPA

MET

HOD

6850

.0

Perchlorate is both naturally occurring and man-made. In its natural

form, perchlorate is a contaminent in fertilizers. Man-made perchlorate is

used in a wide variety of industrial applications including the production

of rubber and paint, in lubricants, and as a primary ingredient in solid

rocket propellant. Perchlorate is highly water soluble and can migrate

into groundwater and surface water, posing a concern to drinking water

supplies. Thirty-five states have detected perchlorate in drinking water

at higher levels than expected. The United States Environmental

Protection Agency (US EPA) has established an official reference dose

of 0.0007 ppb per day of perchlorate. Maryland, Massachusetts and

New Mexico have established a one part per billion (ppb) action

limit, while California and Texas have established 4 ppb limits.

HPlC CoNdiTioNS

Instrument: Alliance® 2695 system with conductivity detector

Column: Waters IC-Pak™ Anion HR, 6 μm , 4.6 x 75 mm

Eluent: 25 mM NH4HCO3, pH 10 with NH4OH in 50% ACN


Column Temp: 30 ˚C

Back Pressure: <1000 psi

Back Conditions: ~1600 μS

Injection: 100 μL

MS CoNdiTioNS

Instrument: Quattro micro™ mass spectrometer

Ionization: ESI- LM 1 Resolution: 15.0

Capillary (V): 0.58 HM 1 Resolution: 15.0

Cone (V): 40 Ion Energy 1: 0.6

Extractor (V): 3 Entrance (V): 1

RF Lens (V): 0.3 Collision Energy: 30

Source Temp ˚C: 125 Exit: 1

Desolvation Temp: 400 LM 2 Resolution: 14.0

Cone Gas (L/hr): 50 HM 2 Resolution: 14.0

Desolvation Gas: 500 Ion Energy 2: 1.0

Gas Cell Pressure: 2 x 10-2 mbar Multiplier: 650

0.5 ppb perchlorate detection in three different sample matrices by LC/MS/MS.



IC-Pak Anion HR, 6 μm, 4.6 x 75 mm WAT026765

Perchlorate Standard 186004155

Perchlorate CRM 186004253




The Determination of Perchlorate in Water Using

LC/MS/MS

720000941EN

The Determination of Perchlorate in Drinking Water

Using Single Quadrupole Mass Spectrometry

720001285EN


Cations &Water Dip

ClRegion

SO4Region

Analyzed on consecutive days with fresh eluent Det Limit at 3x S/N < 0.1 ppb

100 µL of0.5 ppb ClO4

“HTDS”

MilfordDrinking Water

Reagent Water

2 4 6 8 10 12 14 16 18 20. min

Resp

onse

1.2

3 x 1

03

© 2010 Waters Corporation. Waters, The Science of What’s Possible, Alliance, Quattro micro, and IC-Pak are trademarks of Waters Corporation.

perChloraTesDetermination of Perchlorate in Water, Soils and Solid Wastes using High Performance Liquid

Chromatography/Electrospray Ionization/Mass Spectrometry (HPLC/ESI/MS)

30

Polycyclic aromatic hydrocarbons (PAHs) are one of the most

widespread organic pollutants. PAHs are made up of fused aromatic

rings and are formed during the combustion of carbon-based fuels

(wood, coal, diesel), as well as being present in crude oil. The United

States Environmental Protection Agency (US EPA) has classified seven

PAH compounds as being potentially carcinogenic including benz[a]-

anthracene, benzo[a]pyrene, benzo[b]fluoranthene, benzo[k]fluoran-

thene, chrysene, dibenz[a,h]anthracene, and indeno[1,2,3-cd]pyrene.

HPlC CoNdiTioNS

Instrument: Alliance® HPLC system with PDA and fluorescence detectors

Column: Waters PAH, 4.6 x 250 mm @ 30 °C

Eluent: Water/acetonitrile

Injection: 20 μL of Supelco® standard EPA 610 (#48743) diluted

1:50 in 40:60 water/acetonitrile





SAMPlE PrEPArATioN

MeCl2 extraction.

EluENT PrEPArATioN


A: Water

B: Acetonitrile


Initial 1.2 40 60 -

12.0 1.2 0 100 9

23.0 1.2 40 60 11

Eluent gradient.

AnalyteuV

max (nm)

EX (nm)

EM (nm)

detection limit (ppb)1

1 Naphthalene 220 277 330 0.14


3 Acenaphthene 227 270 323 0.01

4 Fluorene 261 265 310 0.03

5 Phenanthrene 251 252 365 0.02

6 Anthracene 252 250 402 0.01

7 Fluoranthene 236 284 467 0.02

8 Pyrene 240 332 378 0.01


10 Chrysene 267 270 367 0.04



13 Benzo(a )pyrene2 296 280 410 0.03



16 Indeno(1,2,3-cd )pyrene 250 305 480 0.491 Fluorescence mode used for detection limit determination, no pre-concentration. Seven replicates per 40 CFR pt. 136 App. B.2 Regulated compound; action level 0.17 ppb.




6 10 14 18 22 min

0.05

AU

1

2

3

4

5

6

7

8

9

10

11

1213

14

15 16

Determination of Polycyclic Aromatic Hydrocarbons in Ground Water and Wastes

EPA

MET

HOD

8310

.0

31

EPA

MET

HOD

8310

.0Determination of Polycyclic Aromatic Hydrocarbons in Ground Water and Wastes


Standard chromatogram, fluorescence/programmed wavelengths, 1-20 ppm PAH analytes.



PAH Column, 4.6 x 250 mm 186001265



The Determination of Biodegradation Products of

PAH Using LC/MS/MS

WA20747

Waters PAH Columns Improve Analysis of

PAH Compounds

720000382EN


© 2010 Waters Corporation. Waters, The Science of What’s Possible, Alliance, and Empower are trademarks of Waters Corporation. Supelco is a registered trademark of Sigma-Aldrich Co.

Determination of Polycyclic Aromatic Hydrocarbons in Ground Water and Wastes

6 10 14 18 22 min

1

3

4

5

6

7

8

9

10 11

1213 14

1516

8000

EU

32

The presence of numerous military and defense sites around the

world, both active and decommissioned, has resulted in the presence

of explosives compounds in locations where they can enter the water

supply. In the US, the evaluation of sites for potential contamination

is carried out by the United States Environmental Protection Agency

(US EPA), US Department of Defense, and US Department of Energy

in support of Superfund, RCRA, and Base Closure environmental

programs.

HPlC CoNdiTioNS

Instrument: Alliance® HPLC system with 2487

Dual λ Absorbance detector

Eluent: 10 mM ammonium formate/isopropanol

Column: XTerra® Phenyl, 3.5 μm, 2.1 x 150 mm @ 40 °C

Injection: 10 μL of standard




SAMPlE PrEPrATioN

Sample Matrix: Groundwater and surface water, low concentration

Sample Prep: Solid-phase extraction using a 500 mL sample Porapak™

reverse-phase sorbent (RDX), elute with acetonitrile

AlTErNATE SAMPlE PrEPArATioN

Oasis® HLB Extraction Method

Oasis HLB Extraction Cartridge, 6 cc, 200 mg

1 This wash step will remove humic and other interferences.2 Tetyl is unstable in base-this step removed NH4OH prior to elution.

STANdArd PrEPArATioN

Dilute 100 μL of AccuStandard® mix (M-8330-R) to 10 mL with

eluent for a working 10 ppm standard mixture.

EluENT PrEPArATioN

10 mM ammonium formate/isoprapanol

Dissolve 0.631 g of ammonium formate in 100 mL water. Transfer

to a 1 L volumetric flask. Add 200 mL of Isopropanol. Dilute to the

mark with water and mix well. Carefully pH to 3.8 with formic acid,

then filter and degas.

explosives

CONDITION/EQUILIBRATE:

4 mL methanol/4 mL water

LOAD:

500-1000 mL sample

WASH:1

2 mL of 5:35:60 NH4OH/methanol/twater

LOAD:

Up to 500 mL sample

RE-EQUILIBRATE:

1 mL water2

AIR DRY:

5 minutes

ELUTE:

2 mL 15:85 water/acetonitrile

Adjust to exactly 5 mL

with 0.1% formic acid in water

Determination of Nitroaromatics and Nitramines by High Performance Liquid Chromatography (HPLC)

EPA

MET

HOD

8330

.0

33

EPA

MET

HOD

8310

.0

© 2010 Waters Corporation. Waters, The Science of What’s Possible, Alliance, XTerra, Empower, Porapak, ACQUITY UPLC, UPLC, and Oasis are trademarks of Waters Corporation. AccuStandard is a registered trademark of AccuStandard Inc.

Standard chromatogram, 10 ppm each analyte.



XTerra Phenyl, 3.5 μm, 2.1 x 150 mm 186001181

Porapak Reverse-Phase Sorbent (RDX) WAT047220

UCMR2 Explosives in Water CRM 186004261


The Science of ACQUITY UPLC® Applied

to Environmental Analyses of PAHs and

Explosives in Water

720001398EN

Explosives in River Water – Oasis Solution WA31764.82

An Improved Method for Determination of

Nitroaromatic and Nitramine Explosives

in Aqueous Samples

WA20717

High Speed Explosives Monitoring using UPLC® 720000950EN


explosives

2 6 10 14 18 22 min

0.25

AU

12

3

4

5

6

7

8

9

10 11

12 13 14

Determination of Nitroaromatics and Nitramines by High Performance Liquid Chromatography (HPLC)


1 HMX 8 2 Amino-4,6 Dinitrotoluene

2 RDX 9 2,4 Dinitrotoluene

3 1,3,5-Trinitrobenzene 10 4 Amino-2,6 Dinitrotoluene

4 1,3 Dinitrobenzene 11 2,6 Dinitrotoluene

5 Nitrobenzene 12 4- Nitrotoluene

6 TNT 13 2- Nitrotoluene

7 Tetryl 14 3- Nitrotoluene

34

© 2010 Waters Corporation. Waters, The Science of What’s Possible, Alliance, XBridge, Empower, and Sep-Pak are trademarks of Waters Corporation. AccuStandard is a registered trademark of AccuStandard Inc.

Formaldehyde is an important industrial chemical used in the manufac-

turing of other chemicals, building materials, and household products.

It is one of the large family of chemical compounds called volatile

organic compounds or “VOCs”. At normal room temperatures these

compounds vaporize. When present in air at levels above 0.1 ppm it can

cause watery eyes, burning sensations in the eyes and nasal passages,

as well as coughing, wheezing, and allergic reactions. Formaldehyde has

been classified as a potential carcinogen and, as such, is regulated in

many countries: Japan, 0.08 ppm; World Health Organization Europe,

0.08 ppm; Sweden, 0.1 ppm; US Department of Housing and Urban

Development, 0.4 ppm.

HPlC CoNdiTioNS

Instrument: Alliance® HPLC system with UV detection

Column: XBridge™ Phenyl, 3.5 μm, 4.6 x 150 mm @ 35 °C

Eluent: Water/tetrahydrofuran/acetonitrile

Injection: 20 μL each of AccuStandard® mix (M- 8315-R1- DNPH and

M- 8315-R2- DNPH) diluted 1:5 in 40:60 water/acetonitrile




SAMPlE PrEPArATioN

Use Sep-Pak® DNPH Silica cartridge, backflush cartridge

with acetonitrile.

EluENT PrEPArATioN

filter and degas through a 0.45 μm filter.

A: 90% water, 10% tetrahydrofuran (THF).

Mix 900 mL water and 100 mL stabilized THF.

B: Acetonitrile


Initial 1.5 70 30 -

20.0 1.5 36 64 6

22.0 1.5 36 64 6

22.1 1.5 70 30 6

Eluent gradient for EPA Methods 554 and 8315 Option 1.


Initial 1.5 70 30 -

16.0 1.5 53 47 6

21.0 1.5 53 47 6

21.1 1.5 70 30 6

Eluent gradient for EPA Methods TO11 and 8315 Option 2.

EPA Method TO11 and 8315-02 analytes, 20 ppm as DNPH analytes.


description Part Number

XTerra Phenyl, 3.5 μm, 2.1 x 150 mm 186001181

Sep-Pak DNPH-Silica Cartridge WAT037500


Determination of Formaldehyde in Ambient Air 720001988EN

Analysis of DNPH Derivatives using

XBridge Phenyl

WAT60186

Reducing Acetronitrile Usage fpr the HPLC

Analysis of Aldehyde and Ketone Pollutants

720003012EN


formaldehyde

1

1514

1312

11

10987

65

4

3

2

0.20

AU

4 6 12 16 20 min

Determination of Formaldehyde in Ambient Air using Adsorbant Cartridge followed by High Performance Liquid Chromatography (HPLC)


1 Formaldehyde 9 Isovaleraldehyde

2 Acetaldehyde 10 Pentanal

3 Acetone 11 o-Tolualdehyde

4 Acrolein 12 p-Tolualdehyde

5 Propanal 13 m-Tolualdehyde

6 Crotonaldehyde 14 Hexanal

7 Butanal 15 2-5 Dimenthylbenzaldehyde

8 Benzaldehyde

EPA

MET

HOD

TO11

Continue...

35

EPA

MET

HOD

555.

0

EPA Method 555 describes the analysis of chlorinated acid pesticides

using HPLC with UV detection. With the PDA Detector, you can utilize

multiple UPLC/MS strategies for the identification of compounds that

are difficult to resolve by conventional HPLC-based methods, detect

and quantify lower concentrations of sample analytes, and compare

spectra across wavelengths and broad concentration ranges.

Compounds that may be analyzed using this method include:

Group A Group B

Picloram 4-Nitrophenol

Chloramben MCPA

Dicamba 3,5- Dichlorobenzoic acid

Bentazon MCPP

2,4-D 2,4,5-T

Dichlorprop 2,4-DB

2,4,5-TP Dinoseb

Acifluorfen Pentachlorophenol

CoNdiTioNS

Instrument: ACQUITY® UPLC

Column: ACQUITY BEH C18, 2.1 x 100 mm, 1.7 μm

Eluent: Binary gradient (see p.37)

Column Temp: 40.7 °C

Injection: 5.0 μL each of AccuStandard® Mix M- 555 (Mix A and B) diluted 1:1000 in 1:1 water/acetonitrile

Weak Wash: 5% Aqueous acetonitrile (800 μL)

Strong Wash: 50% Aqueous acetonitrile (500 μL)


Detection: UV-PDA Scan 210 to 350 nm

SAMPlE PrEPArATioN

EPA

Method Sample Matrix Sample Preparation

555 Ground and finished drinking water

Solid Phase Extraction – Adjust a 75.0-mL water sample to pH 12 with 6 N NaOH. Allow to set for 1 hr, then acidify to pH 2 with H3PO4 and filter. Condition an Oasis® cartridge with 3.0 mL 10:90 methanol/ MTBE, rinse with 2.0 mL MeOH, 2.0 mL water. Load sample, wash with 1.0 mL water, elute with 2.0 mL 10:90 MeOH/MTBE, evaporate to 0.2 mL then recon-stitute to 0.5 mL with water.

EPA Method 555 sample matrix and preparation.

CoMMENTS

Detection limits of <1.0 ppb can be achieved using UV detection.

2,4,5-TP is also known as Silvex®.

5-Hydroxydicamba, listed in method, is no longer available

as a standard.

Use retention time, confirmation wavelengths, and area response.

ratios to confirm analytes. A PDA spectral library can also be created.

Analytes are grouped into two sets A and B and run separately.

EPA Method 555 may be found at the EPA website: www.EPA.gov.

dATA ACQuiSiTioN ANd ProCESSiNg

Data were acquired using Waters Empower™ 2 Software. This system

provides simultaneous 2D and 3D operation in either Empower or

MassLynx™ software.

EluENT PrEPArATioN

A: 25-mM phosphoric acid, pipette 2 mL of 85% H3PO4

into HPLC grade water, and dilute to 1 L.

B: Acetonitrile

Filter and degas through a 0.45 μm PES filter.

ChlorinaTed aCidsACQUITY UPLC System with Photodiode Array (PDA) Detector

36

0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0 3.2 3.4 3.6 3.8 4.0 4.2 min

1

876543

2

8

7

6

54

3

2

1

0.02 AU

0.02 AU

Group A analytes UV at 230 nm

Group B analytes UV at 230 nm

EPA

MET

HOD

555.

0

Time flow (ml/min) %A %B Curve

Initial 0.6 72 28 -

3.7 0.6 37 63 6

4.5 0.6 37 63 6

4.6 0.6 72 28 6

Eluent gradient for EPA Method 555.

EPA Method 555 analytes, Groups A and B (1 ppm).

Analyte and group Confirmation

Wavelength (nm)

Area response

ratio

Acifluorfen (A) 293 1.72Bentazon (A) 240 1.08Chloramben (A) 214 0.612,4-D (A) 285 4.02

2,4-DB (B) 285 5.93

Dicamba (A) 220 0.66

3,5-Dichlorobenzoicacid (B)

285 5.15

Dichlorprop (A) 285 4.07Dinoseb (B) 268 0.48

MCPA (B) 285 6.66MCPP (B) 285 6.494-Nitrophenol (B) 310 0.56

Pentachlorophenol (B)

290 5.65

Picloram (A) 223 0.82

2,4,5-T (B) 290 4.00

2,4,5-TP (A) 293 3.84

Confirmation wavelengths and area response ratios (ARR) for method analytes. ARA=peak area at 230 nm/peak area at confirmation wavelength.

ChlorinaTed aCidsACQUITY UPLC System with Photodiode Array (PDA) Detector

© 2010 Waters Corporation. Waters, The Science of What’s Possible, Oasis, ACQUITY UPLC, MassLynx, ACQUITY, and Empower are trademarks of Waters Corporation. Silvex is a registered trademark of Silberline Manufacturing Co., Inc. AccuStandard is a registered trademark of AccuStandard, Inc.

Peak Analyte1 Picloram2 Chloramben3 Dicamba4 Bentazon5 2,4-D6 Dichlorprop7 2,4,5-TP (Silvex)8 Acifluoren

Peak Analyte1 4-Nitrophenol2 MCPA3 3, 5 Dichlorobenzoic Acid4 MCPP5 2, 4, 5-T6 2, 4-DB7 Dinoseb8 Pentachlorophenol



ACQUITY BEH C18 Column, 1.7 µm, 2.1 x 100 mm 186002352


Continue...

37

Recent research has provided evidence that perfluorinated compounds

(PFCs), such as perfluorooctanesulfonic acid (PFOS) and perfluorooctanoic

acid (PFOA), are persistant organic pollutants and are ubiquitous in the

environment. Because PFCs may be toxic and have bioaccumulative

properties, there is growing interest in the development of analytical

methods for PFCs in the environment.

uPlC CoNdiTioNS

Instrument: ACQUITY UPLC® system

Column: ACQUITY UPLC BEH C18, 1.7 μm, 2.1 x 50 mm


Injection: 10 μL [full loop injection mode]

Column Temp: 40 ˚C

Mobile Phase: A: 20 mM ammonium acetate in

water/acetonitrile [90:10]

B: Methanol/acetonitrile [60:40]

Gradient: 15% - 95% B over 8 minutes

Curve: Linear

MS CoNdiTioNS

Instrument: Quattro Premier™ XE

Ionization Mode: ESI-

Capillary Voltage: 3 kV

MS Mode: MRM

Desolvation Temp: 350 ˚C

Source Temp: 150 ˚C

PfC MrM Transition Cone (V) Collision (eV)

PFBS 299>80 40 30

PFOS 499>80 50 40

C3 163>119 20 13

C4 213>169 15 10

C5 263>219 15 9

C6 313>269 15 12

C7 363>319 15 10

C8 413>369 15 10

C9 463>419 15 10

C10 513>469 15 10

C11 563>519 15 10

C12 613>569 15 10

Optimized MRM transition parameters.

UPLC®/MS/MS of 12 PFCs spiked at 10 μg/kg in chicken liver.

Oasis® WAX Sorbent and SPE protocol for water and tissue.

perfluorinaTed Compounds (pfC /pfos/pfoa)

PF BS

C3

C4 C5

C6

C7 C8

C9

C10 C11

C12

PF OS

1 0 2 3 4 5 6 7 8 min

2: MRM of 10 Channels ES-

6.16e4

1: MRM of 2 Channels ES-

298.7 > 79.7 + 498.7 > 98.8 8.27e3

TIC

NO

N

NH

N

NH

H

H+

+

pKa ~60.6 meq/g

Oasis WAX PREPARED SAMPLE:

pH 3-5

CONDITION:

2 mL of methanol/2 mL water

LOAD:

100 mL water or 20 mL diluted

tissue extract

WASH 1:

1 mL 2% Formic Acid

ELUTE 1 (WASH 2):

2 mL methanol

ELUTE 2:

2 mL 1% ammonia in MTB:

methanol (90:10)*

* Alternatively use 2 mL of

1% ammonia in methanol

Emerging Contaminant of Concern

C3= Perfluoropropanoic acid C7= Perfluoroheptanoic acid C10= Perfluorodecanoic acid

C4= Perfluorobutyric acid C8= Perfluorooctanoic acid C11= Perfluoroundecanoic acid

C5= Perfluoropentanoic acid C9= Perfluorononanoic acid C12= Perfluorododecanoic acid

C6= Perfluorohexanoic acid

PFBS = Pefluorobutanesulfonic acid

PFOS = Perfluorooctanesulfonic acid

38

perfluorinaTed Compounds (pfC /pfos/pfoa)

© 2010 Waters Corporation. Waters, The Science of What’s Possible, Oasis, ACQUITY UPLC, UPLC, ACQUITY, and Quattro Premier are trademarks of Waters Corporation.

SAMPlE PrEPArATioN

Method 1: Water

Water samples [100 mL] were spiked with the appropriate compounds,

adjusted to pH 3 with formic acid, and then processed by SPE. The

SPE eluate [Elute 2] was collected in polypropylene test tubes, diluted

with 2 mL of 2% aqueous formic acid and brought to 5 mL with water.

Alternatively, the eluate may be evaporated and reconstituted in

mobile phase prior to analysis, but polypropylene labware should

be used exclusively.

Method 2: Tissues

A 1 mL aliquot of supernatant was diluted to 20 mL with water and the

pH was adjusted to 4-5 using 2% formic acid. This solution was then

loaded on an Oasis® WAX cartridge. SPE eluates were evaporated and

reconstituted in 1 mL of mobile phase [polypropylene labware].

Spike level μg/l PfBS PfoS C3 C4 C5 C6 C7 C8 C9 C10 C11

0.10 122 109 108 119 97 184 107 83 121 101 101

0.30 110 117 95 132 105 110 119 126 137 118 94

0.70 102 98 91 107 93 118 100 78 103 126 119

1.0 113 94 128 106 98 130 100 88 100 110 117

4.0 104 86 101 99 99 102 102 92 115 99 84

10 104 100 98 101 100 87 89 82 103 99 101

Recovery of PFCs from drinking water.


description Part Number

ACQUITY® BEH C18, 1.7 μm, 2.1 x 50 mm 186002350

Oasis WAX, 3 cc, 60 mg 186002492




Analysis of Perfluorinated Compounds (PFCs)

on the ACQUITY UPLC System and the Quattro

Premier XE in ES-MS/MS

720001761EN

Separation of Branched PFOS Isomers by UPLC with

MS/MS Detection

720001694EN

Oasis WAX Sorbent for UPLC/MS Determination of

PFOS and Related Compounds in Water and Tissue

720001817EN

Analysis of Perfluorinated Compounds using UPLC

and MS/MS Detection

720001848EN



Continue...

39

Understanding the occurrence, fate, and impact of persistent organic

pollutants (POPs) is a global priority and consequently is undertaken

by a diverse range of organizations. Perfluorinated compounds (PFCs)

have become increasingly important and perfluorooctane sulphonic

acid (PFOS) has been included in the Stockholm Convention on POPs.1

The tracking of PFCs is critical to organizations whose activities

might inadvertently facilitate exposure to populations through

water, food supplies, and consumer products. This is also a priority

for researchers and regulators and is especially true when taking into

account the high publicity related to newer contaminants such as PFCs.

This application note describes advanced high-sensitivity Xevo™ TQ

MS analysis of PFCs in environmental waters and biota, incorporat-

ing dual scan-MRM to understand the nature of the sample matrix,

while simultaneously performing routine quantitation.

SAMPlE PrEPArATioN

Environmental water samples were obtained from Lake Mariestadssjön,

River Svartån, and various drinking water sources in Sweden. Fish liver

samples were from unknown locations in Norway.

Method for Oasis® Wax, 6 cc, 150 mg catridge

uPlC CoNdiTioNS

Instrument: ACQUITY UPLC® with PFC Analysis Kit

Column: ACQUITY® BEH C18 column, 2.1 x 50 mm, 1.7 μm

Column Temp: 50 ˚C

Mobile Phase: A: (98:2) 2 mM CH3COONH4 (aqueous):MeOH

B: MeOH + 2 mM CH3COONH4


Injection: 10 μL

Gradient: Time (min) Flow Rate %A %B

Initial 0.65 75 25

0.50 0.65 75 25

5.00 0.65 15 85

5.10 0.65 0 100

6.60 0.65 0 100

6.70 0.65 7 25

MS CoNdiTioNS

MS System: Xevo TQ MS

Acquisition Mode: Dual Scan-MRM (DS-MRM)

Ionization Mode: ESI -

Capillary Voltage: 0.44 kV

Source Temp: 150 °C

Desolvation Temp: 600 °C

Desolvation Gas: 900 L/hr

Cone Gas Flow: 30 mL/min

Collision Gas Flow: 0.18 mL/min

Overlaid MRM chromatograms of each target PFC (solvent standard; concentrations range between 1 pg/μl and 2 pg/μl).

perfluorinaTed CompoundsAdvancing Perfluorinated Compounds Analysis Using Simultaneious Matrix Monitoring

CONDITION:

4 mL 0.1% NH4OH/MeOH, 4 mL MeOH, 4 mL H20

LOAD SAMPLE:

Under vacuum between 3 mL/min and 6 mL/min

DRY:

Under vacuum

WASH:

Acetate buffer (4 mL, 0.025 M), 4 mL MeOH

ELUTE:

4 mL 0.1t% NH4OH/MeOH

Eluent was evaporated and reconstituted to 40:60 MeOH:H20

with 2 mM ammonium acetate. The final extracts were filtered or

centrifuged if necessary.PFBuS

PFHxA

PFHpAPFHxS

THPFOS

PFOA

PFOS

PFNA

PFDA

PFUnDA

PFDoDA

PFBuS

PFHxA

PFHpAPFHxS

THPFOS

PFOA

PFOS

PFNA

PFDA

PFUnDA

PFDoDA

4 0



Oasis WAX, 6 cc, 150 mg 186002493

ACQUITY PFC Column Kit 176001692

ACQUITY PFC Analysis Kit 176001744


ACQUITY UPLC System for Quantifying Trace Levels

of Perfluorinated Compounds with an ACQUITY PFC

Analysis Kit

720002813EN

Advancing Endocrine Disrupting Compound Analysis

through Integrated Technology and Workflow Solutions

720003013EN


perfluorinaTed CompoundsAdvancing Perfluorinated Compounds Analysis Using Simultaneious Matrix Monitoring

© 2010 Waters Corporation. Waters, The Science of What’s Possible, Xevo, Oasis, ACQUITY UPLC, ACQUITY, and UPLC are trademarks of Waters Corporation. Excerpt from Waters Application Note 720003162EN.

Tap Water

Tap Water Lake Mariestadssjön River Svartån

Compound name: PFOACorrelation coefficient: r = 0.999898, r^2 = 0.999796Calibration curve: 0.311728 * x + 0.0612933Response type: Internal Std ( Ref 6 ), Area * ( IS Conc. / IS Area )Curve type: Linear, Origin: Exclude, Weighting: Null, Axis trans: None

Conc

0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0 16.0

Resp

onse

0.00

1.00

2.00

3.00

4.00

5.00

Compound name: PFOSCorrelation coefficient: r = 0.999705, r^2 = 0.999410Calibration curve: 0.558744 * x + 0.0416708Response type: Internal Std ( Ref 11 ), Area * ( IS Conc. / IS Area )Curve type: Linear, Origin: Exclude, Weighting: Null, Axis trans: None

Conc0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0 16.0 18.0 20.0

Resp

onse

0.0

2.0

4.0

6.0

8.0

10.0

413 > 369

413 > 219

413 > 169

Lake Mariestadssjön River Svartån

499 > 99

499 > 80

Quantitative data for PFOA (top) and PFOS (bottom), including calibration curves and extracted MRM chromatograms. Native concentrations in tap water (PFOA 0.42 ng/L, PFOS 1.50 ng/L), Lake Mariestadssjön (PFOA 1.30 ng/L, PFOS 1.30 ng/L), and River Svartån (PFOA 1.10 ng/L, PFOS 1.40 ng/L).

Continue...

41

Emerging evidence from wildlife and laboratory studies indicates

that some chemicals may interfere with the endocrine system.

Compounds identified as endocrine-disrupting chemicals (EDCs)

include pesticides, polychlorinated biphenyls (PCBs), dioxins,

furans, alkylphenols, and steroid hormones.

HPlC CoNdiTioNS

Instrument: Alliance® 2690 HPLC system

Column: SunFire™ C18, 3.5 μm, 2.1 x 50 mm

Mobile Phase A: Methanol

Mobile Phase B: Water


Injection volume: 20 μL

Gradient: Time (min) %A %B

Initial 60 40

10 100 -

18 100 -

20 60 40

23 60 40

MS CoNdiTioNS

A Waters Quattro micro™ triple quadrupole mass spectrometer was

operated in the negative ion electrospray mode. Nitrogen gas, at a

flow rate of 450 L/hr and a temperature of 250 °C, was used for spray

desolvation. The source temperature was maintained at 120 °C and the

capillary voltage was 3.2 kV.

Compound fwPrecursor ion m/z

Product ions m/z

Corresponding structure of product ions

Cone Voltage (V)

Collision Energy (eV)

Estriol 288.4 287.3 144.9; 171.1 [M - C8H14O2]-; [M - C6H12O2] 50 40

Bisphenol A 228.3 227.2 133.0; 210.8 [M - C6H6O]- 37 33

17α-Ethinylestradiol 296.4 295.5 145.1; 199.5 [M - C10H14O]-; [M - C6H9O]- 37 49

17α-Estradiol 272.4 271.3 145.2; 183.1 [M - C10H14O]-; [M - C5H12O]- 37 45

17β-Estradiol 272.4 271.3 145.2; 183.1 [M - C8H14O]-; [M - C5H12O]- 37 45

Estrone 270.4 269.2 144.8; 143 [M - C8H12O]-; [M - C8H14O]- 37 33

4-n-Nonylphenol 220.4 219.3 106.0; 118.7 [M - C8H17]-; [M - C7H17]- 40 34

Pentachlorophenol 266.3SIR of 264.9263.0; 267.1;

269.040 -

MRM parameters.

SAMPlE PrEPArATioN

Method for Oasis® HLB, 3 cc, 60 mg

endoCrine disrupTorsEmerging Contaminant of Concern

CONDITION:

3 mL Methyl t-butyl ether (MTBE) 3 mL Methanol (MeOH)

3 mL ultra-high quality water

LOAD:

500 mL acidified river water

SAMPLE:

10 mM formate buffer pH=3.0

WASH:

3 mL 40% MeOH in UHQ water 3 mL UHQ water 3 mL

10% MeOH/2% NH4OH in water

ELUTE:

6 mL 10% MeOH/MTBE

EVAPORATE:

To dryness by gentle stream of nitrogen at 50 °C

RE-DISSOLUTION:

500 μL (50:50, v/v, acetonitrile/tammonium formate buffer pH 3.0)

42

© 2010 Waters Corporation. Waters, The Science of What’s Possible, SunFire, Oasis, Alliance, and Quattro micro are trademarks of Waters Corporation.

The presence of bisphenol A and estron in unspiked river water samples. Spiked river water samples.



SunFire C18 Column, 3.5 μm, 2.1 x 50 mm 186002533





A Sensitive Method for the Determination of

Endocrine-Disrupting Compounds in River Waters

by LC/MS/MS

720001296EN

Determination of Endocrine Disrupting Compounds

(EDCs) in River Water by ACQUITY UPLC Tandem

Quadrupole MS

720002335EN

Endocrine Disruptors – General SPE Guidelines oasis73


endoCrine disrupTors

min

min


Continue...

43

Endocrine disrupting compounds (EDCs) have caused increased concern

for organizations that monitor their occurrence in environmental and

potable waters. These compounds often have physiological effects to

humans and wildlife at very low concentrations.1 One class of EDCs

are the estrogenically active substances. These, of course, include

natural and synthetic estrogens as well as alkylphenol compounds

that mimic at the estrogenic, receptor.2 There is a need to monitor

these compounds reliably to low parts per trillion (ppt) concentrations

in often complex samples such as environmental surface waters and

treated sewage.

This application note describes the use of Waters Oasis® HLB sample

preparation in combination with Xevo™ TQ MS for the analysis of

endocrine disrupters to low ppt concentrations in groundwater, river

water, and sewage effluent. It also describes the use of intelligent

workflow tools for method development, as well as advanced LC/MS/MS

analysis using Dual Scan-MRM.

SAMPlE PrEPArATioN

Method for Oasis HLB, 3 cc, 60 mg

uPlC CoNdiTioNS

Instruments: ACQUITY UPLC®

Run Time: 5.30 min

Column: ACQUITY® BEH C18 1.7 μm, 2.1 x 50 mm

Column Temp: 40˚C

Mobile Phase: A: 0.05% NH4OH (aqueous)

B: MeOH


Injection: 10 μL

Gradient: Time (min) Flow Rate %A %B

Initial 0.60 65.0 35.0

3.00 0.60 5.0 95.0

4.20 0.60 5.0 95.0

4.30 0.60 65.0 35.0

MS CoNdiTioNS

MS System: Xevo TQ

Acquisition Mode: Dual Scan-MRM

Ionization Mode: ESI

Capillary Voltage: 2.0 kV

Source Temp: 150 °C

Desolvation Temp: 650 °C

Desolvation Gas: 1100 L/hr

Cone Gas Flow: 20 mL/min

Collision Gas Flow: 0.18 mL/min

endoCrine disrupTorsAdvancing Endocrine Disrupting Compound Analysis through Integrated Technology and Workflow Solutions

CONDITION:

3 mL Methyl t-butyl ether (MTBE) 3 mL Methanol (MeOH)

3 mL ultra-high quality water

LOAD:


SAMPLE:


WASH:

3 mL 40% MeOH in UHQ water 3 mL UHQ water 3 mL

10% MeOH/2% NH4OH in water

ELUTE:

6 mL 10% MeOH/MTBE

EVAPORATE:


RE-DISSOLUTION:

500 μL (50:50, v/v, acetonitrile/ammonium formate buffer pH 3.0)

4 4

Groundwater (A), river water (B), and sewage effluent (C) spiked concentration at 1 ng/mL (equivalent to 5 ng/L with Oasis HLB preconcentration) with the exception of Bisphenol A with native concentrations at 3 ng/L (A), 2 ng/L (B), and 15 ng/L (C).

ordEriNg iNforMATioNrelated Parts Part Number

Oasis HLB glass, 3 cc, 60 mg WAT094226

ACQUITY BEH C18, 1.7 µm, 2.1 x 50 mm 186002350




Through Integrated Technology and Workflow Solutions

720003013EN

A Sensitive Method for the Determination of Endocrine-

Disrupting Compounds in River Water by LC/MS/MS

720001296EN


(EDCs) in River Water by ACQUITY UPLC Tandem

Quadrupole MS/MS

720002335EN

Endocrine Disruptors- General SPE Guidelines oasis73


endoCrine disrupTorsAdvancing Endocrine Disrupting Compound Analysis through Integrated Technology and Workflow Solutions

© 2010 Waters Corporation. Waters, The Science of What’s Possible, UPLC, ACQUITY UPLC, ACQUITY, Oasis, and Xevo are trademarks of Waters Corporation.Excerpt from Waters Application Note 720003013EN.

Continue...

45

Emerging evidence from wildlife and laboratory studies indicates

that some chemicals may interfere with the endocrine system.

Compounds identified as endocrine-disrupting chemicals (EDCs)

include pesticides, polychlorinated biphenyls (PCBs), dioxins,

furans, alkylphenols, and steroid hormones (natural and synthetic).

The steroid hormones are of special concern due to their potency.

The natural sex hormone estradiol and its metabolites (estroneand

estriol) and the synthetic steroid ethinylestradiol are excreted in the

urine of mammals and can be found in surface and ground waters.

Other EDCs, such as the alkylphenols–nonylphenol, bisphenol A and

pentachlorophenol are derived from industrial and domestic activities

and also occur in environmental waters. Bisphenol A is used in the

production of epoxy resins and polycarbonate plastics which are

used extensively in the manufacture of food and drink packaging

materials. Nonylphenol, which is produced as a derivative of non-ion-

ic surfactants, is used extensively as a plasticizer. Pentachlorophenol

is still used in some countries as a heavy-duty wood preservative.

This application note describes a sensitive method for the simultaneous

determination of eight endocrine-disrupting compounds in river water

samples based on SPE followed by LC/MS/MS.

SAMPlE PrEPArATioN

Oasis® HLB Cartridge, 5 cc, 200 mg

HPlC CoNdiTioNS

Instrument: Alliance® 2690

Column: SunFire™ C18, 2.1 x 50 mm with 3.5 μm particle size

Mobile Phase A: Methanol

Mobile Phase B: Water


Injection: 20 μL

Gradient Time (min) %A %B

0 60 40

10 100 0

18 100 0

20 60 40

23 60 40

endoCrine disTrupTors

A Sensitive Method for the Determination of Endocrine-Disrupting Compounds in River Water by LC/MS/MS

CONDITION:

3 mL Methyl t-butyl ether (MTBE) 3 mL Methanol (MeOH) 3 mL

ultra-high quality water

LOAD:


SAMPLE:


WASH:

3 mL 40% MeOH in UHQ water

3 mL UHQ water

3 mL 10% MeOH/2% NH4OH in water

ELUTE:

6 mL 10% MeOH/MTBE

EVAPORATE:


RE-DISSOLUTION:

500 μL (50:50, v/v, acetonitrile/ammonium formate buffer pH 3.0)

4 6

Chromatograms showing peaks close to the instrument LoDs.

The presence of bisphenol A and estron in unspiked river water samples.

Spiked river water samples.



Oasis HLB glass, 5 cc, 200 mg 186000683

SunFire C18, 3.5 µm, 2.1 x 50 mm 186002533




Through Integrated Technology and Workflow Solutions

720003013EN

A Sensitive Method for the Determination of

Endocrine-Disrupting Compounds in River Water by

LC/MS/MS

720001296EN


(EDCs) in River Water by ACQUITY UPLC® Tandem

Quadrupole MS/MS

720002335EN

Ecstacy (MDMA) and Metabolites by LC-MS/MS oasis72


endoCrine disTrupTors

A Sensitive Method for the Determination of Endocrine-Disrupting Compounds in River Water by LC/MS/MS

© 2010 Waters Corporation. Waters, The Science of What’s Possible, Oasis, SunFire, ACQUITY UPLC, and Alliance are trademarks of Waters Corporation. Excerpt from Waters Application Note 720001296EN.

47

Nerve agents are among the most lethal of chemical warfare agents.

In particular, the G-series nerve agents are of a concern due to their

toxicity (LD50 human for GB 25 mg/kg, GD 5 mg/kg, GF 5 mg/kg),

their environmental persistence (hydrolysis half-life of 1-3 days),

their accessibility and their recent use in Iraq and Japan. The poten-

tial use of these agents by terrorist organizations is of real concern and

the ability to counter such attacks requires recognizing possible deploy-

ment scenarios, including the poison¬ing of drinking water supplies.

This report will describe the use of a LC-MS method for the unambigu-

ous identification of six AMPAs in drinking water. The analysis was

performed by LC-ESI-MS and utilized an XBridge™ C18 HPLC column for

chromatographic separation.

HPlC CoNdiTioNS

Instrument: Alliance® 2690

Column: XBridge C18, 2.1 x 150 mm, 3.5 μm

Mobile Phase: 10 mM ammonium formate in water (solvent A)

10 mM ammonium formate in methanol (solvent B)

Elution Gradient: 99% A (0-2 min), 99-30% A (2-17 min),

30% A (17-25 min)


Injection: 5 μL

MS CoNdiTioNS

Instrument: LCT time-of-flight mass spectrometer

with standard Z-spray electrospray interface

ESI Conditions: ESI-

Capillary Voltage: – 2 kV

Sample Cone Voltage: 10 V

Extraction Cone Voltage: 5 V

Desolvation Temp: 300 ˚C

Source Temp: 120 ˚C

Flow Rate: 540 L/h

LC-ESI-MS total ion current chromatograms of seven chemical warfare agents degradation products: (a) XBridge C18 3.5 μm. Compounds: (1) methylphosphonic acid; (2) ethyl methylphosphonic acid; (3) isopropyl methylphosphonic acid; (4) isobutyl methylphosphonic acid; (5) cyclohexyl methylphosphonic acid; (6) pinacolyl methylphosphonic acid; (7) benzilic acid. Chromatogram courtesy of Dr. Jian-wei Xie, Beijing Institute of Pharmacology and Toxicology.



XBridge C18, 3.5 µm, 2.1 x 150 mm 186003023



Determination of Nerve Agent Degradation Products in

Drinking Water

WA60199


nerve agenTs Determination of Nerve Agent Degradation Products in Drinking Water

© 2010 Waters Corporation. Waters, The Science of What’s Possible, Alliance, and XBridge are trademarks of Waters Corporation. Excerpt from Waters Application Note WA60199.

2 4 6 8 10 12 14 16 18 20 min0

100

%

TOF MS ES-TIC

2.88e4

10.91

3.072.27

1.97

10.19

7.17

12.74

17.9118.81

(a)

4 8

EU council directive 76/464/EC1 lists 132 compounds that have

restricted levels in drinking and surface waters. Of these compounds,

109 are amenable to gas chromatographic analysis. Currently pub-

lished methods involve the use of two injections, one using selected

ion recording as a screen, followed by a full scan injection for

confirmation. The use of tandem quadrupole GC/MS/MS allows the

analyst to combine the screening and confirmatory injections into one

run, while also allowing a reduction of the chromatographic separa-

tion required for confirmation of some of the target compounds. The

European Union (EU) list has many similarities with the target compound

lists of United States Environmental Protection Agency (US EPA) water

quality methods such as 6253 and 82704 (it should be noted that the

list analyzed in this method is by no means an exhaustive one). The

compound groups represent a wide range of polarities and compound

types, and include benzidines, chloronitrotoluenes, organochloro pes-

ticides, organophosphorus pesticides, chloroanilines, chlorophenols,

chlo¬ronitrobenzenes, chlorotoluidines, phenylurea pesticides, PCBs,

semi-volatile halogenated compounds, PAHs (Polynuclear Aromatic

Hydrocarbons), triazines and volatile amines.

Combining these groups into a single method would allow the laboratory

to significantly increase sample throughput. The high selectivity and

specificity of multiple reaction monitoring (MRM) acquisitions also help

to shorten the time required for data processing by reducing the possibil-

ity of false positives and time spent confirming the presence of target

compounds. The method presented is intended as an example of what

is possible by implementing techniques such as GC tandem quadrupole

MS/MS and solid phase extraction.

SAMPlE PrEPArATioN

Oasis® HLB 3cc, 60 mg

The GC temperature ramps employed were:

30 m DB17-ms 40 °C/1 min, 3 °C/min to 160 °C, 7 °C/min to

240 °C, 15 °C/min to 305 °C, hold 15 mins. 1 mL/min He flow

40m RTX5 40 ° C/1 min, 3 °C/min to 160 °C, 7 °C/min to

240 °C, 15 °C/min to 310 °C, hold 15 mins. 0.7 ml/min He flow

30 m vf5-ms 40 °C/0.8 min, 6 °C/min to 160 °C, 8 °C/min to

310 °C, hold 2 mins. 0.9 mL/min He flow

All injections in pulsed splitless mode were made with an injection

temperature of 250 °C, using a double gooseneck 4 mm i.d. liner and

1 μL injection volume. The injections were made with a 1 min 110 kPa

pulse, a purge time of 1 minute and a purge flow of 70 mL/min.

Cool on column injections were made in track oven mode.

Data were acquired with MassLynx™ software and processed with

TargetLynx™ Application Manager.

prioriT y polluTanTs

Multi-Residue Analysis of Priority Pollutants in Drinking and Surface Waters Using Solid Phase Extraction and GC Tandem Quadrupole MS/MS

SAMPLE:

Adjust to pH4 using 1 N HCl solution

CONDITION:

6 mL DCM, 6 mL acetonitrile and 6 mL of water at a

flow rate of 3 mL/min

LOAD:

Sample with flow rate of ca 6 mL/min

WASH:

1 mL water

DRY:

Under a flow of nitrogen (ca 1 mL/min) for 20 mins

ELUTE:

A) 2.5 mL DCM/ACN (4:1), 5 mL DCM; or B) 5 mL DCM

EXTRACT:

Adjusted to a volume of ca 0.5 ml under a stream of dry

nitrogen at ambient temperature, add of 500 ng of d10-anthracene

as a recovery standard.

Continue...

49



100

%

0

Reconstructed TIC for all compounds analyzed using DB17-ms column with COC injection.

Critical pairs separation when analyzed using the DB17-ms column with COC injection.

m i n

3 3 .7 0 3 3 .8 0 3 3 .9 0 3 4 .0 0 3 4 .1 0 3 4 .2 0 3 4 .3 0 3 4 .4 0 3 4 .5 0 3 4 .6 0 3 4 .7 0 3 4 .8 0 3 4 .9 0 3 5 .0 0 3 5 .1 0 3 5 .2 0 3 5 .3 0 3 5 .4 0 3 5 .5 0 3 5 .6 0

0

mevinphos (z)31_01_05_COC_12

31_01_05_COC_12

Mevinphos (E)

0

%

33.70 33.80 33.90 34.00 34.10 34.20 34.30 34.40 34.50 34.60 34.70 34.80 34.90 35.00 35.10 35.20 35.30 35.40 35.50 35.60 min

5 1 .2 5 0 5 1 .3 0 0 5 1 .3 5 0 5 1 .4 0 0 5 1 .4 5 0 5 1 .5 0 0 5 1 .5 5 0 5 1 .6 0 0 5 1 .6 5 0 5 1 .7 0 0 5 1 .7 5 0 5 1 .8 0 0 5 1 .8 5 0

%

p, p'-DDD

o, p'-DDT

0

%

51.25 51.30 51.35 51.40 51.45 51.50 51.55 51.60 51.65 51.70 51.75 51.80 51.85 min

100

100

Reconstructed TIC for all compounds analyzed using the vf5-ms column with pulsed splitless injection.

100

%

0

Critical pairs separation when analyzed using the vf5-ms column with pulsed splitless injection.

1 6 .8 0 1 7 .0 0 1 7 .2 0 1 7 .4 0 1 7 .6 0 1 7 .8 0 1 8 .0 0 1 8 .2 0 1 8 .4 0 1 8 .6 0 1 8 .8 0 1 9 .0 0 1 9 .2 0 1 9 .4 0 1 9 .6 0 1 9 .8 0 2 0 .0 0 2 0 .2 0 2 0 .4 0 2 0 .6 0 2 0 .8 0

%

0

3 1 .0 0 3 1 .1 0 3 1 .2 0 3 1 .3 0 3 1 .4 0 3 1 .5 0 3 1 .6 0 3 1 .7 0 3 1 .8 0 3 1 .9 0 3 2 .0 0 3 2 .1 0

%

mevinphos (z)

Mevinphos (E)

o, p'-DDT

p, p'-DDD%

0

16.80 17.00 17.20 17.40 17.60 17.80 18.00 18.20 18.40 18.60 18.80 19.00 19.20 19.40 19.60 19.80 20.00 20.20 20.40 20.60 20.80 min

31.00 31.10 31.20 31.30 31.40 31.50 31.60 31.70 31.80 31.90 32.00 32.10 min

100

%

0

100

50



Optimized MRM transitions for analytes and internal/recovery standards.

Compound MrM 1 CE MrM 2 CE

1,2-Dichloronaphthalene 196 > 126 25 196 > 161 15

1-Chloro-2,4-dinitrobenzene 202 > 107 10 202 > 79 10

1-Chloro-3-nitrobenzene 157 > 111 10 157 > 75 25

1-Chloro-4-nitrobenzene 157 > 99 10 157 > 75 25

2,3,4-Trichlorophenol 196 > 97 25 198 > 97 25



2,3-Dichloroaniline 161 > 90 15 161 > 125 10

2,3-Dichloronitrobenzene 145 >109 10 191 > 109 27




2,4-Dichloronitrobenzene 145 > 109 10 191 > 109 27

2,4-Dichlorophenol 162 > 63 20 164 > 63 20




2-Chloro-3-nitrotoluene 171 > 77 12 171 > 113 10

2-Chloro-4-toluidine 141 > 106 12 141 > 77 30


2-Chloroaniline 127 > 65 15 127 > 100 10

2-Chlorophenol 128 > 64 15 128 > 100 10

2-Fluorobiphenyl [Internal STD] 172 > 151 20 - -

3,3'-Dichlorobenzidine 252 > 154 25 252 > 127 45






3-Chloroaniline 127 > 65 15 127 > 100 10

3-Chlorophenol 128 > 65 15 128 > 100 5


4-Chloro-3-methylphenol 142 > 107 10 142 > 77 25

4-Chloro-3-nitroltoluene 171 > 77 12 171 > 113 10

4-Chloroaniline 127 > 65 15 127 > 100 10

4-Chlorophenol 128 > 65 15 128 > 100 5

Continue...

51

Aldrin 263 > 193 25 293 > 186 30

Alpha-chlordane 372.9 > 265.9 20 372.9 > 300.9 7

Alpha-endosulfan 241 > 206 10 241 > 170 20

Alpha-hexachlorocyclohexane 219 > 183 8 181 > 145 10

Anthracene 178 > 152 15 178 > 151 40

Atrazine 200 > 122 10 200 > 94 15

Azinphos-ethyl 160 > 132 5 160 > 77 15

Azinphos-methyl 160 > 132 5 160 > 77 15

Bentazone 198 > 119 10 198 > 92 25

Benzidine 184 > 156 18 184 > 139 32

Benzo[a]pyrene 252 > 250 30 252 > 224 47

Benzo[b]fluoranthene 252 > 250 30 252 > 224 47

Benzo[ghi]perylene 276 > 274 40 276 > 272 55

Benzo[k]fluoranthene 252 > 250 30 252 > 224 47

Beta-endosulfan 241 > 206 10 241 > 170 20

Beta-hexachlorocyclohexane 219 > 183 8 181 > 145 10

Biphenyl 154 > 152 20 154 > 102 30

Coumaphos 362 > 109 15 362 > 334 5

Cumene 120 > 105 7 120 > 77 25

d10-anthracene [recovery STD] 188.1 > 160 20 - -

d5-nitrobenzene [Internal STD] 128 > 82 10 - -

Delta-hexachlorocyclohexane 219 > 183 8 181 > 145 10

Demeton-o 171 > 115 10 171 > 143 5

Demton-s-methyl 142 > 112 6 230 > 88 6

Dibenz(a,h)anthracene 278 > 276 40 278 > 274 55

Dichlorvos 185 > 93 10 220 > 185 5

Dieldrin 344.9 > 263 15 279 > 243 10

Dimethoate 229 > 87 7 229 > 86 20

Disulfoton 274 > 88 5 186 > 142 5

Endrin 263 > 193 30 263 > 191 30

Fenitrothion 277 > 109 15 277 > 127 15

Fenthion 278 > 109 15 278 > 79 30

Fluoranthene 202 > 200 30 202 > 150 45

Gamma-chlordane 372.9 > 265.9 20 372.9 > 300.9 10

Heptachlor 272 > 237 10 272 > 142.9 30

Hexachlorobenzene 283.8 > 248.9 15 285.8 > 213.8 25

Compound MrM 1 CE MrM 2 CE


(continued)



52

Hexachlorobutadiene 225 > 190 13 260 > 225 10

Indeno(1,2,3-cd)pyrene 276 > 274 40 276 > 272 55

Isodrin 193 > 123 25 263 > 193 25

Lindane 219 > 183 8 181 > 145 10

Linuron 248 > 61 10 250 > 61 8

Malathion 173 > 99 10 173 > 127 5

Mevinphos(E) 192 > 127 10 192 > 164 5

mevinphos(Z) 192 > 127 10 192 > 164 5

Monolinuron 126 > 99 10 214 > 61 10

Naphthalene 128 > 102 15 128 > 78 15

o,o'-DDE 246 > 176 21 318 > 248 18

o,o'-DDE 246 > 176 21 318 > 248 18

o,p-DDD 235 > 165 20 237 > 165 20

o,p'-DDT 235 > 165 20 237 > 165 20

Omethoate 156 > 110 7 156 > 79 20

p,p'-DDD 235 > 165 20 237 > 165 20

p,p'-DDE 246 > 176 21 318 > 248 18

p,p'-DDT 235 > 165 20 237 > 165 20

Parathion-ethyl 291 > 109 12 291 > 81 35

Parathion-methyl 263 > 109 10 263 > 127 10

PCB#101 325.9 > 255.9 25 327.9 > 255.9 25

PCB#118 325.9 > 255.9 25 327.9 > 255.9 25

PCB#126 325.9 > 255.9 25 327.9 > 255.9 25

PCB#138 359.8 > 289.9 25 361.8 > 289.9 25

PCB#153 359.8 > 289.9 25 361.8 > 289.9 25

PCB#169 359.8 > 289.9 25 361.8 > 289.9 25

PCB#180 393.8 > 323.9 22 395.8 > 323.9 22

PCB#28 256 > 186 15 258 > 186 15

PCB#52 289.9 > 220 23 291.9 > 220 23

PCB#77 289.9 > 220 23 291.9 > 220 23

Pentachlorophenol 265.8 > 166.9 20 267.8 > 166.9 20

Phenanthrene 178 > 152 15 178 > 151 40

Propanil 217 > 161 10 161 > 126 15

p-Terphenyl-d14 [Internal STD] 244.1 > 226 20 - -

Pyrazon 221 > 77 15 221 > 105 10

Simazine 201 > 173 6 201 > 138 10


Compound MRM 1 CE MRM 2 CE

(continued)



53

Tetrachloronaphthalene 265.9 > 196 25 265.9 > 194 25

Triazophos 257 > 162 7 257 > 119 22

Tributyl Phosphate 155 > 99 5 211 > 99 10

Trifluralin 306 > 264 10 306 > 160 20

Compound MRM 1 CE MRM 2 CE


(continued)

Recovery Range 70-120% 50-70% <50% >120%

Elution A 36% 27% 14% 24%

Elution B 72% 8% 13% 7% Summary of extraction recoveries, expressed as percentage of total number of compounds within each range. Based upon average of five replicates.



Oasis HLB glass, 3 cc, 60 mg WAT094226



Multi-Residue Analysis of Priority Pollutants in Drinking

and Surface Waters Using Solid Phase Extraction and GC

Tandem Quadrupole MS/MS

720001438EN


0 2 0 4 0 6 0 8 0 1 0 0 1 2 0

160

140

120

100

80

60

40

20

00 20 40 60 80 100 120

Compound number

Distribution of average recoveries (n=5) for elution method B (5 mL DCM).

© 2010 Waters Corporation. Waters, The Science of What’s Possible, Oasis, MassLynx, and TargetLynx, are trademarks of Waters Corporation. Excerpt from Waters Application Note 720001438EN.



54

WATErS AlliANCE HPlC SySTEM

The Alliance® HPLC systems offer flexibility with easy-to-configure instrumentation modules that address the needs of multiple applications. Alliance is built around the 2695 Separations Module, which offers integrated solvent and sample management. The 2695 Separations Module is designed to work with both MassLynx™ mass spectrometry and Empower™ 2 chromatography software, the complete range of Waters HPLC column chemistries and a variety of Waters high performance detectors, including photodiode array (PDA), multi-wave-length fluorescence and dual-wavelength absorbance.

feaTured sysTems

WATErS ACQuiTy uPlC SySTEM

The ACQUITY UPLC® system features a novel liquid chromatography technology that uses 1.7 μm stationary phase pressure-tolerant particles. When combined with high pressure fluidic modules, a fast response detector and integrated data analysis software, UPLC® technology delivers faster run times, better resolution and greater sensitivity.

WATErS AlliANCE SySTEM for CArBAMATE ANAlySiS

The Alliance HPLC system for carbamate analysis is a completely integrated system that detects carbamate at parts-per-trillion levels necessary for regulatory compliance, and exceeds precision and accuracy requirements mandated by the United States Environmental Protection Agency (US EPA) and Association of Official Analytical Chemists (AOAC) methods. The analysis of glyphosate can also be performed on the same system.

55

WATErS QuATTro MiCro APi MASS SPECTroMETEr

The Waters Quattro micro™ API incorporates the finest high-precision tandem quadrupole mass analyzer technology in only 15.3 in (390 mm) of linear bench space. The mass analyzer has a standard m/z range of 2 to 2000 and a sensitivity equivalent to systems that are three times the size.

feaTured sysTems

WATErS ACQuiTy uPlC SySTEM WiTH THE TQ dETECTor

The ACQUITY TQD is a smaller, easier to use, enhanced capability tandem quadrupole mass detector specifically designed as an afford-able, fast MS/MS system compatible with UPLC. Labs will benefit from robust and reliable performance and walk-up operation. Interactive IntelliStart™ diagnostics software allows for worry-free system optimization and performance checks.

ACQuiTy uPlC H-ClASS SySTEM

Access the productivity and chromatographic performance of UPLC with the familiarity of HPLC. Laboratories can now have UPLC results with a system that combines the flexibility of ternary or quaternary solvent blending with the simplicity of flow-through needle injec-tions. You can even continue running your existing HPLC methods with this forward looking platform and seamlessly transition to UPLC separations when you're ready.

56

WaTers spe soluTions

In addition to our complete Environmental Analysis Solutions, Waters also supplies solid-phase extraction tools which can be used with a

wide number of EPA methods. Featuring our revolutionary Oasis and classic Sep-Pak technologies, we can assist you by providing fast, reliable, and

compliant extractions of your environmental samples. For your convenience, we have listed EPA methods and the corresponding Waters SPE

cartridges below in the form of two Quick Reference Charts.

SPE Solutions reference Chart

EPA Method Number SPE Siorbent

504 Sep-Pak Silica

506 Sep-Pak C18

507 Sep-Pak C18

508.1 Sep-Pak C18

513 Sep-Pak C18

525 Sep-Pak C18/Oasis HLB

532 Sep-Pak C18

535 Oasis HLB

547 Oasis MAX

548 Sep-Pak C18/Oasis HLB

549 Sep-Pak C8/Oasis WCX

550.1 Sep-Pak C18

552.1 Oasis HLB/Oasis MAX

553 Sep-Pak C18

554 Sep-Pak Silica

555 Sep-Pak Silica

608 Sep-Pak C18

625 Oasis HLB

629 Oasis HLB

632 Oasis MCX

1613 Sep-Pak C18

1614 Sep-Pak C18

1657 Sep-Pak C18

1668 Sep-Pak C18

1694 Sep-Pak C18

8080 Sep-Pak C18

8082 Sep-Pak C18

8315a Sep-Pak C18

8318a Oasis HLB

8330 Pora-Pak RDX

8440 Sep-Pak Silica

TO-11A Sep-Pak DNPH

Emerging Contaminants

PFOS, PFOA Oasis WAX

Pharmaceutical Compounds Oasis HLB

Endocrine Disruptors Oasis HLB

EPA Method Number

430 636

506 638

509 639

515.1 645

606 646

607 1656

608.2 1658

609 8032

611 8061

614 8080

617 8081

619 8111

622.1 8121

629 8131

632 8141

633.1

For a complete listing of our Environmental Analysis

products, visit www.waters.com/environment to

download the following materials:

Environmental Analysis Catalog

Literature code: 720002639EN

florisil SPE Quick reference Chart

Sorbent Selection Guide for



Environmental Analysis

Solutions Brochure


57

QuiCK referenCe guides

WATErS CErTifiEd rEfErENCE MATEriAlS ANd QC STANdArdS SoluTioNS

With the addition of Environmental Resource Associates (ERA) to the

Waters family, we are pleased to provide a wide range of Certified

Reference Materials (CRMs) and QC Standards for your environmental

testing needs. Based upon the highest levels of technical and

manufacturing excellence, these products ensure accurate and

compliant results. For your convenience, we have listed the analytical

techniques and EPA methods (as well as several other widely utilized

methods) supported by our CRM and QC standards offering in the

form of a quick reference chart.

CErTifiEd rEfErENCE MATEriAlS/QC STANdArdS QuiCk rEfErENCE CHArT

Waters is pleased to be able to provide Certified Reference Materials

and/or QC Standards for the following analytical techniques:

Atomic Absorption Spectrometry (AA)

Colorimetric

Inductively Coupled Plasma - Optimcal Emmission Spectroscopy (ICP-OES)

Inductively Coupled Plasma - Mass Spectrometry (ICP-MS)

Ion Chromatography (IC)

Infrared Spectroscopy (IR)

Gravimetric

Nephelometric

Titrimetric

Ion - Selectivity Electrodes (ISE)

Distillation

Purge and Trap

Whole Effluent Testing (WET)

Gas Chromatography (GC)

High Performance Liquid Chromatography (HPLC)

UltraPerformance Liquid Chromatography (UPLC)

Resource Conservation and Recovery Act Methods (RCRA)

Superfund Methods

EPA METHodS

oTHEr METHodS

EPA Method Number

5 413.1 548 8091

5a 413.2 549 8141

5b 418 550 8151

5d 418.1 551 8260

5f 425.1 552 8270

6 502.2 555 8280

7 504 608 8290

8 505 610 8310

0010 506 613 8318

13a 507 614 8330

12 508 619 8440

14 508a 622 9071B

26 508.1 625 CTM 027

26a 515.1 632 TO-04A

29 515.2 633 TO-10A

0030 515.3 1613 TO-11A

0031 515.4 1664 TO-13A

0061/7119 521 3050 TO-14

101A 524.2 3051 TO-15

110.1 525 4020 TO-17

110.2 525.2 5520

110.3 529 8015

160.4 531.1 8021

200.8 535 8081

331.2 547 8082

other Methods

ASTM D5673-03

California ELAP Requirements

CARB Method 425

Long Term 2 Enhanced Surface Water Treatment Rule

SDWA Quantitative Methods

Standard Method 2120B

Standard Method 2120C

Standard Method 2120E

Standard Method 2540E

Standard Method 3125



58

EU Number Name of Priority SubstanceOasis HLB Cartridges

240-110-8 Alachlor 60 mg/3 mL

240-110-8 Alachlor 60 mg/3 mL

204-371-1 Anthracene 200 mg/6 mL

217-617-8 Atrazine 200 mg/6 mL

207-432-0 Chlorfenvinphos 200 mg/6 mL

220-864-4 Chlorpyrifos 200 mg/6 mL

204-211-0 Di[2-ethylhexyl]phthalate[DEHP] (also bis[ethylhexyl] phthalate)

200 mg/6 mL

206-354-4 Diuront 200 mg/6 mL

204-079-4 Endosulfan 60 mg/3 mL

N/A Alpha-endosulfan 60 mg/3 mL

205-912-4 Fluoranthene 200 mg/6 mL

204-273-9 Hexachlorobenzene 60 mg/3 mL

201-765-5 Hexachlorobutadiene 60 mg/3 mL

210-158-9 Hexachlorocyclohexane 60 mg/3 mL

200-401-2 Gamma-isomer, Lindane 60 mg/3 mL

251-835-4 Isoproturon 200 mg/6 mL

202-049-5 Naphthalene 200 mg/6 mL

246-672-0 Nonylphenols 200 mg/6 mL

203-199-4 4-[para]-nonylphenol 200 mg/6 mL

217-302-5 Octylphenols 200 mg/6 mL

N/A (4-[1,1’,3,3’-tetramethylbutyl]-phe-nol) (AKA para-tert-octylphenol)

200 mg/6 mL

210-172-5 Pentachlorobenzene 60 mg/3 mL

231-152-8 Pentachlorophenol (PCP) 60 mg/3 mL

N/A Polyaromatic hydrocarbons 200 mg/6 mL

200-028-5 Benzo[a]pyrene 200 mg/6 mL

205-911-9 Benzo[b]fluoranthene 200 mg/6 mL

205-883-8 Benzo[g,h,i]perylene 200 mg/6 mL

205-916-6 Benzo[k]fluoranthene 200 mg/6 mL

205-893-2 Indeno[1,2,3-cd]pyrene 200 mg/6 mL

204-535-2 Simazine 60 mg/3 mL

216-428-8 Trifluralin 60 mg/3 mL

Sep-Pak Cartridges

211-704-4 Tributyltin compounds C18

Oasis HLB Cartridges

211-704-4 Tributyltin compounds C18

EuroPEAN uNioN WATEr frAMEWork dirECTiVE – SPE SoluTioNS

QuiCK referenCe guides

59

SEP-PAk CArTridgESTitle Author(s) Institution(s) Journal Citation

Cytotoxic and Genotoxic Potential of Drinking Water: A Comparison between Two Different Concentration Methods

Annamaria Buschini, Federica Giordani, Claudia Pellacani, Carlo Rossi and Paola Poli

Dipartimento di Genetica, Biologia dei Microrganismi, Antropologia, Evoluzi-one, Università di Parma, Via Usberti, 11/A, 43100 Parma, Italy

Water Research Volume 42, Issues 8-9, April 2008, Pages 1999-2006

Simultaneous Analysis of 16 Sulfon-amide and Trimethoprim Antibiotics in Environmental Eaters by Liquid Chromatography–electrospray Tandem Mass Spectrometry

Hong Chang, Jianying Hu, Mari Asami and Shoichi Kunikane

College of Urban and Environmental Sciences, Peking University, Beijing 100871, China; Department of Water Supply Engineering, National Institute of Public Health, Saitama 351-0197, Japan

Journal of Chromatography A Volume 1190, Issues 1-2, 9 May 2008, Pages 390-393

Reduction in Microcystin Concentra-tions in Large and Shallow Lakes: Water and Sediment-Interface Contributions

Wei Chen, Lirong Song, Liang Peng, Neng Wan, Xiaoming Zhang and Nanqin Gan

State Key Laboratory of Freshwater Ecology and Biotechnology, Institute of Hydrobiology, The Chinese Academy of Sciences, Wuhan 430072, PR China; Graduate School of Chinese Academy of Sciences, Beijing 100049, PR China

Water Research Volume 42, Issue 3, February 2008, Pages 763-773

Evaluation of a Multiresidue Method for Measuring Fourteen Chemical Groups of Pesticides in Water by Use of LC-MS-MS

J. J. Carvalho, P. C. A. Jerónimo, C. Gonçalves and M. F. Alpen-durada

IAREN-Water Institute of the Northern Region, Rua Dr. Eduardo Torres, 229, 4450–113 Matosinhos, Portugal; FFUP-Faculty of Pharmacy, University of Porto, Laboratory of Hydrology, Rua Aníbal Cunha 164, 4050–047 Porto, Portugal

Analytical and Bioanalytical Chemistry, Issue Volume 392, Number 5 / November, 2008, Pages 955-968

Solid-Phase Extraction and LC with Fluorescence Detection for Analysis of PAHs in Rainwater

O. Delhomme, E. Rieb and M. Millet

Laboratoire de Physico-Chimie de l’Atmosphère (UMR 7517), Centre de Géochimie de la Surface et Département de Chimie de l’Université Louis Pasteur, 1 rue Blessig, 67084 Strasbourg Cedex, France

Chromatographia, Issue Volume 65, Numbers 3-4 / February, 2007, Pages 163-171

Analysis of Nitroaromatic Compounds in Complex Samples Using Solid-phase Microextraction and Isotope Dilution Quantification Gas Chroma-tography–electron-capture Negative Ionisation Mass Spectrometry

S. Jönsson, L. Gustavsson and B. van Bavel

Man–Technology–Environment Research Centre, Department of Natural Sci-ences, Örebro University, 701 82 Örebro, Sweden

Journal of Chromatography A Volume 1164, Issues 1-2, 14 September 2007, Pages 65-73

Simultaneous Determination of the Endocrine Disrupting Compounds Non-ylphenol, Nonylphenol Ethoxylates, Triclosan and Bisphenol A in Waste-water and Sewage Sludge by Gas Chromatography–mass Spectrometry

Georgia Gatidou, Nikolaos S. Tho-maidis, Athanasios S. Stasinakis and Themistokles D. Lekkas

Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Panepistimioupolis Zografou, 15771 Athens, Greece; Water and Air Quality Laboratory, Department of Environmental Studies, University of the Aegean, University Hill, 81100 Mytilene, Greece

Journal of Chromatography A Volume 1138, Issues 1-2, 5 January 2007, Pages 32-41

Simultaneous Analysis of 16 Sulfon-amide and Trimethoprim Antibiotics in Environmental Waters by Liquid Chromatography–electrospray Tandem Mass Spectrometry

Hong Chang, Jianying Hu, Mari Asami and Shoichi Kunikane

College of Urban and Environmental Sciences, Peking University, Beijing 100871, China; Department of Water Supply Engineering, National Institute of Public Health, Saitama 351-0197, Japan


Distribution and Fluxes of Fluorescent Whitening Agents Discharged from Domestic Wastewater Into Small Rivers with Seasonal Changes of Flow Rates

Kazuhide Hayakawa, Ryouji Okumura, Hiroki Yamamoto, Manabu Fujiwara, Nobuhisa Yamaji, Hideshige Takada, Ma-sakazu Kanematsu and Yoshihisa Shimizu

Lake Biwa Environmental Research Institute, 5-34 Yanagasaki, Otsu, Shiga 520-0022, Japan; Department of Material Chemistry, Ryukoku University, Shiga, Japan; Faculty of Agriculture, Tokyo University of Agriculture and Tech-nology, Tokyo, Japan; Research Center for Environmental Quality Management, Kyoto University, Shiga, Japan

Limnology, Issue Volume 8, Number 3 / December, 2007, Pages 251-259

Existence of Nonpoint Source of Perfluorinated Compounds and Their Loads in the Tsurumi River Basin, Japan

Yasuyuki Zushia, Tomoharu Takedaa and Shigeki Masunaga

Graduate School of Environment and Information Sciences, Yokohama National University, 79-7 Tokiwadai, Hodogaya-ku, Yokohama, Kanagawa 240-8501, Japan

Chemosphere Volume 71, Issue 8, April 2008, Pages 1566-1573

Occurrence of Sulfonamide Antibiotics in Sewage Treatment Plants

Chang Hong, Hu JianYing, Wang LeZheng and Shao Bing

College of Environmental Sciences, Peking University, Beijing, 100871, China; Beijing Center for Disease Prevention and Control, Beijing, 100013, China

Chinese Science Bulletin, Issue Volume 53, Number 4 / February, 2008, Pages 514-520

Occurrence of a Veterinary Antibiotic in Streams in a Small Aatchment Area with Livestock Farms

Yoshihiko Matsui, Takahiro Ozu, Takanobu Inoue and Taku Matsushita

Hokkaido University, Graduate School of Engineering, Sapporo 060-8628, Japan; Gifu University, Department of Civil Engineering, Gifu 501-1193, Japan; Toyohashi University of Technology, Department of Architecture and Civil Engineering, Toyohashi 441-8580, Japan

Desalination Volume 226, Issues 1-3, 25 June 2008, Pages 215-221

seleCTed published referenCes

60

Sample Preparation of Sewage Sludge and Soil Samples for the Determina-tion of Polycyclic Aromatic Hydrocar-bons Based on One-pot Microwave-assisted Saponification and Extraction

M. Teresa Pena, Luis Pensado, M. Carmen Casais, M. Carmen Mejuto and Rafael Cela

Dpto. Química Analítica, Nutrición y Bromatología. Instituto de Investigación y Análisis Alimentario, Universidad de Santiago de Compostela, 15782 Santiago de Compostela, Spain

Analytical and Bioanalytical Chemistry, Issue Volume 387, Number 7 / April, 2007, Pages 2559-2567

Optimization of the Matrix Solid-phase Dispersion Sample Preparation Procedure for Analysis of Polycyclic Aromatic Hydrocarbons in Soils: Comparison with Microwave-assisted Extraction

M.T. Pena, M.C. Casais, M.C. Mejuto and R. Cela

Dpto. Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario, Universidad de Santiago de Compostela, 15782 Santiago de Compostela, Spain


Preconcentration of Pharmaceuticals Residues in Sediment Samples Using Microwave Assisted Micellar Extraction Coupled with Solid-phase Extraction and their determination by HPLC-UV

R. Cueva-Mestanza, Z. Sosa-Ferrera, M.E. Torres-Padrón and J.J. Santana-Rodríguez

Department of Chemistry, Faculty of Marine Sciences, University of Las Palmas de Gran Canaria, 35017 Las Palmas de Gran Canaria, Spain

Journal of Chromatography B Volume 863, Issue 1, 15 Febru-ary 2008, Pages 150-157

Multiresidue Determination of Pesti-cides in Sediment by Ultrasonically Assisted Extraction and Gas Chroma-tography/Mass Spectrometry

Kuniaki Kawata, Takashi Asada, Kikuo Oikawa, Akiko Tanabe

Journal of AOAC INTERNATION-AL, Volume: 88 | Issue: 5, Page(s): 1440-1451

Isotopic Signature of Nitrate in Two Contrasting Watersheds of Brush Brook, Vermont, USA

Heidi C. Hales, Donald S. Ross and Andrea Lini

Department of Environmental Conservation, 103 S. Main St., Waterbury, VT 05671, USA; Department of Plant and Soil Science, University of Vermont, Burlington, VT 05405, USA; Department of Geology, University of Vermont, Burlington, VT 05405, USA

Biogeochemistry, Issue Volume 84, Number 1 / May, 2007, Pages 51-66

13C NMR Study of the Effect of Aero-bic Treatment of Olive Mill Wastewater (OMW) on its Lipid-free Content

H. El Hajjouji, G. Merlina, E. Pinelli, P. Winterton, J.-C. Revel and M. Hafidi

Equipe d’Ecologie Végétale, Sol et Environnement, Département de Biologie, Faculté des Sciences Semlalia, Université Cadi Ayyad, BP 2390, Marrakech, Morocco; Ecole Nationale Supérieure Agronomique de Toulouse, EcoLab, UMR 5245 CNRS-UPS-INPT, Avenue de l’Agrobiopôle, BP 32607, Auzeville Tolo-sane, 31326 Castanet-Tolosan, France; Université Paul Sabatier, 118 Route de Narbonne, 31062 Toulouse Cedex, France

Journal of Hazardous Materials Volume 154, Issues 1-3, 15 June 2008, Pages 927-932

SEP-PAk rdXTitle Author (s) Institution(s) Journal Citation

New Hydrophilic Materials for Solid-phase Extraction

N. Fontanals, R.M. Marcé and F. Borrull

Departament de Química Analítica i Química Orgánica, Universitat Rovira i Virgili, Campus Sescelades, Marcel·lí Domingo, s/n, E-43007 Tarragona, Spain

TrAC Trends in Analytical Chem-istry Volume 24, Issue 5, May 2005, Pages 394-406

RDX and TNT residues from live-fire and blow-in-place detonations

Alan D. Hewitt, Thomas F. Jen-kins, Marianne E. Walsh, Michael R. Walsh and Susan Taylor

US Army Engineer Research and Development Center, Cold Regions Research and Engineering Laboratory, Hanover, NH 03755-1290, USA

Chemosphere Volume 61, Issue 6, November 2005, Pages 888-894

RDX Biodegradation Column Study: Comparison of Electron Donors for Biologically Induced Reductive Transformation in Groundwater

Jeffrey L. Davisa, Altaf H. Wan, Brenda R. O’Nealb and Lance D. Hansen

Environmental Laboratory, US Army Engineer Research and Development Center (Attn: CEERD-EP-E), 3909 Halls Ferry Road, Vicksburg, MS 39180, USA; Applied Research Associates, Inc., Southern Division, 119 Monument Place, Vicksburg, MS 39180, USA

Journal of Hazardous Materials Volume 112, Issues 1-2, 9 August 2004, Pages 45-54

Trace Level Analysis of Hexahydro-1,3,5-Trinitro-1,3,5-Triazine (RDX) and its Biodegradation Intermedi-ates in Liquid Media by Solid-phase Extraction and High-pressure Liquid Chromatography Analysis

Chow TM, Wilcoxon MR, Piwoni MD, Adrian NR.

The Illinois Waste Management Research and Information Center, Champaign, IL 61820, USA.

J Chromatogr Sci. 2004 Oct;42(9):470-3

Determination of 3,3'-Dichlorobenzi-dine in Industrial Wastewaters

Lee, Hing-Biu, Peart, T E, Terry, K and Maguire, R J

Water Quality Research Journal of Canada. Vol. 39, no. 1, Pages 29-34. 2004

Analysis of Nitroaromatic Compounds in Complex Samples Using Solid-phase Microextraction and Isotope Dilution Quantification Gas Chroma-tography-electron-capture Negative Ionization Mass Spectrometry

S. Jönsson, L. Gustavssona and B. van Bavel

Man–Technology–Environment Research Centre, Department of Natural Sci-ences, Örebro University, 701 82 Örebro, Sweden


Title Author(s) Institution(s) Journal Citation


61

Extraction Properties of New Poly-meric Sorbents in SPE/GC Analysis of Phenol and Hydroquinone from Water Samples

Katarzyna Bielicka-Daszkiewicz, Adam Voelkela, Monika Szejnera and Joanna Osypiuk

Institute of Chemical Technology and Engineering, Poznań University of Technology, Pl. M. Skłodowskiej-Curie 2, 60-965 Poznań, Poland; Division of Chemistry and Polymer Technology, M. Curie-Skłodowska University, ul. Gliniana 33, 20-614 Lublin, Poland

Chemosphere Volume 62, Issue 6, February 2006, Pages 890-898

Comparison of Solid-phase Extraction Sorbents for Sample Clean-up in the Analysis of Organic Explosives

Romain Tachona, Valérie Pichon, Martine Barbe Le Borgnea and Jean-Jacques Minet

Laboratoire Central de la Préfecture de Police, 39 bis rue de Dantzig, 75015 Paris, France; Laboratoire Environnement et Chimie Analytique (UMR CNRS 7121), École Supérieure de Physique et Chimie Industrielles, 10 rue Vauquelin, 75231 Paris Cedex 05, France

Journal of Chromatography A Volume 1185, Issue 1, 21 March 2008, Pages 1-8

Determination of Explosives in Environmental Water Samples by Solid-phase Microextraction–liquid Chromatography

Fanny Monteil-Riveraa, Chantale Beaulieua, Stéphane Deschampsa, Louise Paqueta and Jalal Hawari

Biotechnology Research Institute, National Research Council of Canada, 6100 Royalmount Avenue, Montreal, Que., H4P 2R2 Canada

Journal of Chromatography A Volume 1048, Issue 2, 10 Sep-tember 2004, Pages 213-221

Biologically Mediated Reductive Transformation of Ordnance Related Compounds by Mixed Aquifer Culture Using Acetate as the Sole Carbon Source: Laboratory Treatability Studies for Field Demonstration

Altaf H. Wani and Jeffrey L. Davis Senior Environmental Engineer, Applied Research Associates, Inc., 119 Monument Place, Vicksburg, MS. E-mail: [email protected]; Leader, Organics Remediation Research Team, Environmental Laboratory, U.S. Army Engineer Research and Development Center, 3909 Halls Ferry Road, Vicksburg, MS.

Pract. Periodical of Haz., Toxic, and Radioactive Waste Mgmt. Volume 10, Issue 2, pp. 86-93 (April 2006)

Comparison of TNT Removal from Seawater by Three Marine Macroalgae

Octavio Cruz-Uribe, Donald P. Cheney and Gregory L. Rorrer

Department of Chemical Engineering, Oregon State University, Corvallis, OR 97331, USA; Department of Biology, Northeastern University, Boston, MA 02115, USA

Volume 67, Issue 8, April 2007, Pages 1469-1476

Remediating RDX-Contaminated Ground Water with Permanganate

M. L. Adama, S. D. Comfortb, M. C. Morleya and D. D. Snow

Department of Civil Engineering, University of Nebraska, Lincoln, NE 68588-0531; School of Natural Resources, University of Nebraska, Lincoln, NE 68583-0915; Water Science Laboratory, University of Nebraska, Lincoln, NE 68583-0844

J. Environ. Qual. 33:2165-2173 (2004).

Dynamic Preconcentration of Organic Substances on Nonpolar Adsorbents

O. A. Filippov, T. I. Tikhomirova, G. I. Tsizin and Yu. A. Zolotov

Department of Chemistry, Moscow State University, Leninskie gory, Moscow, 119899, Russia

Journal of Analytical Chemistry, Issue Volume 58, Number 5 / May, 2003, Pages 398-422

SEP-PAk dNPHTitle Author(s) Institution(s) Journal Citation

Utilization of Solid-phase Extraction (SPE) for the Determination of Polycyclic Aromatic Hydrocarbons in Environmental Aqueous Matrices

Rivelino M. Cavalcante; Nilton S. M. Filho; Rommel B. Viana; Isadora R. N. Oliveira; Ronaldo F. Nascimento, Edilberto R. SilveiraI; George S. S. Freire

Departamento de Química Analítica e Físico Química, Universidade Federal do Ceará, Av. Humberto Monte, s/n, 60455-760 Fortaleza – CE, Brasil; Depar-tamento de Química Orgânica e Inorgânica, Universidade Federal do Ceará, CP 12200, 60451-970 Fortaleza – CE, Brasil; Departamento de Geologia, Universidade Federal do Ceará, Fortaleza – CE, Brasil

Quím. Nova vol.30 no.3 São Paulo May/June 2007

Trends of Ambient Carbonyl Com-pounds in the Urban Environment of Hong Kong

Della W. M. Sin, Yiu-Chung Wong and Peter K. K. Louie

Air Chemistry Section, Analytical & Advisory Division, Government Laboratory, 7th fl, Ho Man Tin Govt Office, 88 Chung Hau Street, Homantin, Hong Kong Special Administrative Region (HKSAR), Kowloon, Hong Kong; Air Services Group, Environmental Protection Department, Revenue Tower, 5 Gloucester Road, Wanchai, HKSAR, Hong Kong

Atmospheric Environment Volume 35, Issue 34, December 2001, Pages 5961-5969

Atmospheric Alcohols and Aldehydes Concentrations Measured in Osaka, Japan and in Sao Paulo, Brazil

Ha Thi-Hoang Nguyen, Norimichi Takenaka, Hiroshi Bandow, Yasuaki Maeda, Sergio T. de Oliva, Maria M. f. Botelho and Tania M. Tavares

College of Engineering, Osaka Prefecture University, 1-1 Gakuen-cho, Sakai, Osaka, 599-8531, Japan; Instituto de Quimica,Universidade Federal da Bahia, CEP 40170-280, Salvador, Bahia, Brazil

Atmospheric Environment Volume 35, Issue 18, June 2001, Pages 3075-3083

Importance of Handling Organic Atmospheric Pollutants for Assessing Air Quality

C. Borrego, P. Gomesa, N. Barros and A. I. Mirand

Institute for Environment and Development (IDAD), University of Aveiro, 3810-193 Aveiro, Portugal; Department of Environment and Planning, University of Aveiro, 3810-193 Aveiro, Portugal

Journal of Chromatography A Vol-ume 889, Issues 1-2, 11 August 2000, Pages 271-279

Seasonal and Diurnal Variations of Carbonyl Compounds in Beijing Ambient Air

Xiaobing Pang and Yujing Mu State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China

Atmospheric Environment Volume 40, Issue 33, October 2006, Pages 6313-6320

Investigation and Estimation of Emis-sion Sources of 54 Volatile Organic Compounds in Ambient Air in Tokyo

Jun-ya Hoshia, Saeko Amano, Yuko Sasaki and Takashi Ko-renaga

Tokyo Metropolitan Research Institute for Environmental Protection, 1-7-5 Shin-suna Koto, Tokyo 136-0075, Japan; Department of Chemistry, Graduate School of Science, Tokyo Metropolitan University, 1-1 Minami-Ohsawa, Hachioji, Tokyo 192-0397, Japan

Atmospheric Environment Volume 42, Issue 10, March 2008, Pages 2383-2393



62

VOC and Carbonyl Emissions from Carpets: A Comparative Study Using Four Types of Environmental Chambers

Athanasios Katsoyiannis, Paolo Levaa and Dimitrios Kotzias

European Commission (EC), Joint Research Center (JRC), Institute for Health and Consumer Protection (IHCP), Physical and Chemical Exposure Unit (PCE), Ispra (Va), TP-281, Via E. Fermi 1, I-21020, Italy

Journal of Hazardous Materials Volume 152, Issue 2, 1 April 2008, Pages 669-676

SEP-PAk XPoSurETitle Author(s) Institution(s) Journal Citation

Levels and Determinants of Formalde-hyde, Acetaldehyde, and Acrolein in Residential Indoor Air in Prince Edward Island, Canada

Nicolas L. Gilbert, Mireille Guay, J. David Miller, Stan Judek, Ceci-lia C. Chan and Robert E. Dales

Air Health Effects Division, Health Canada, 400 Cooper Street, PL 4602C, Ottawa, Ont., Canada K1A 0K9; Department of Chemistry, Carleton University, 1125 Colonel By Drive, Ottawa, Ont., Canada K1S 5B6; Cassen Testing Laboratories, 211-215 Carlingview Drive, Toronto, Ont., Canada M9W 5X8; Department of Medicine, The Ottawa Hospital, 501 Smyth Road, Box 211, Ottawa, Ont., Canada K1H 8L6

A Passive Sampler for the Determina-tion of Carbonyl Compounds in Indoor Air Employing O-(4-cyano-2-ethoxy-benzyl) Hydroxylamine as Reactive Adsorbent

Masayuki Onishi, Yoshika Sekine, Koichi Sugihara, Kazuya Kitasaka and Hatsumi Shimajiri

Department of Chemistry, School of Science, Tokai University; Osaka Labora-tory, Sumika Chemical Analysis Service, Ltd.

Journal of Health ScienceVolume 53 (2007) , No. 4, Pages 413-422

Concentrations of Ethene and Formal-dehyde at a Valley and a Mountain Top Site in the Austrian Alps

S. Smidt, H. Bauer, O. Pogodina-band H. Puxbaum

Federal Office and Research Centre for Forests (BFW Vienna), Seckendorff-Gudent Weg 8, 1131 Vienna, Austria; Vienna University of Technology, Institute for Chemical Technologies and Analytics, Getreidemarkt 9/164UPA, 1060 Vienna, Austria

Atmospheric EnvironmentVolume 39, Issue 22, July 2005, Pages 4087-4091

Assessment of the Emission Characteristics of VOCs from Interior Furniture Materials during the Con-struction Process

S.K. Pang, Hyun Cho, J.Y. Sohn, K.D. Song

Indoor and Built Environment, Volume 16, No. 5, Pages 444-455 (2007)

Organic Air Pollutants Inside and Outside Residences in Shimizu, Japan: Levels, Sources and Risks

Takeshi Ohura, Takashi Amagai, Yoshinori Senga and Masahiro Fusaya

Institute for Environmental Sciences, University of Shizuoka, 52-1 Yada, Shizuoka 422-8526, Japan; Shizuoka Institute of Environment and Hygiene, 4-27-2 Kita-ando, Shizuoka 420-8637, Japan

Science of The Total EnvironmentVolume 366, Issues 2-3, 1 August 2006, Pages 485-499

Field Validation of an Active Sampling Cartridge as a Passive Sampler for Long-Term Carbonyl Monitoring

Naohide Shinohara, Kazukiyo Kumagai; Naomichi Yamamoto, Yukio Yanagisawa, Minoru Fujii, Akihiro Yamasaki

Journal of the Air & Waste Management Association, 2004, Volume 54 (No.4)

Development of a Ppb-level Sensor Based on Catalytic Combustion for Total Volatile Organic Compounds in Indoor Air

T. Sasahara, H. Kato, A. Saito, M. Nishimura and M. Egashira

Research and Technology Center, Yazaki Corp., Susono-shi, Shizuoka 410-1194, Japan; Faculty of Engineering, Nagasaki University, Nagasaki-shi, Nagasaki 852-8521, Japan

Sensors and Actuators B: Chemical Volume 126, Issue 2, 1 October 2007, Pages 536-543

SEP-PAk AC2Title Author(s) Institution(s) Journal Citation

Determination of 1,4-Dioxane in Household Detergents and Cleaners

Akiko Tanabe and Kuniaki Kawata Niigata University of Pharmacy and Applied Life Sciences, Faculty of Pharma-ceutical Sciences, 265-1 Higashijima, Akiha-Ku, Niigata 956-8603, Japan; Niigata University of Pharmacy and Applied Life Sciences, Faculty of Applied Life Sciences, 265-1 Higashijima, Akiha-Ku, Niigata 956-8603, Japan.

Journal of AOAC International, Volume: 91 | Issue: 2, February 2008, Pages 439-444

Study on the Screening Method of Chemicals in Leachate Samples by Solid-phase Extraction and LC/MS Analysis

Uebori Michiko, Imamura Kiyoshi, Ishii Yoshiaki, Hasegawa Atsuko, Yoshida Yasuko, Suzuki Shigeru

Environmental Conservation Engineering, Volume 35; No. 8; Pages 588-595 (2006)

Simulataneous Determination of Acephate, Omethoate and Meth-amidophos by LC/MS in Agricultural Products

Suzuki Keiko, Tsuboi Hiroshi, Miyashita Taeko, Fujita Kozo

Annual Report of Sapporo City Institute of Public Health, Volume; No. 33; Pages 57-62 (2006)

Simple Automated Preparation of O-[11C]methyl-l-tyrosine for Routine Clinical Use

Yoichi Ishikawa, Ren Iwata, Shozo Furumoto, Claudio Pascali, Anna Bogni, Kazuo Kubota and Kiichi Ishiwata

CYRIC Tohoku University, Aramaki, Aoba-ku, Sendai 980-8578, Japan; TU-BERO, Tohoku University, Sendai 980-8575, Japan; National Cancer Institute, 20133 Milan, Italy; International Medical Center, Tokyo 162-8655, Japan; Tokyo Metropolitan Institute of Gerontology, Tokyo 173-0022, Japan

Applied Radiation and Isotopes-Volume 63, Issue 1, July 2005, Pages 55-61



63

Determination of Hexaconazole in Surface Water Samples from River and the Sea by Liquid Chromatog-raphy-Electrospray Tandem Mass Spectrometry

Hiroko Tsukatani, Kazuhiro Tobiishi, Yoshito Tanaka, Kenji Sakuragi Tasoh Ikeura and Matayoshi Nakamura

Fukuoka Institute of Health and Environmental Sciences Bioscience, Biotechnology, and Biochemistry, Volume 72 (2008), No. 1; Pages 149-154

Determination of Amitrole in Environ-mental Water Samples by LC/MS/M

Uebori Michiko Journal of Environmental Chem-istry, Volume 13; No. 2; Pages 445-452 (2003)

SEP-PAk PS2Title Author(s) Institution(s) Journal Citation

Determination of Nitroarenes in Precipitation Collected in Kanazawa, Japan

Tsuyoshi Murahashi, Misao Ito, Ryoichi Kizu and Kazuichi Hayakawa

Japan Automobile Research Institute, 2530 Karima, Tsukuba-shi, 305-0822, Japan; Faculty of Pharmaceutical Sciences, Kanazawa University, 13-1 Takara-machi, Kanazawa-shi, 920-0934, Japan

Water Research, Volume 35, Issue 14, October 2001, Pages 3367-3372

Determination and Quantitation of Sulfonylurea and Urea Herbicides in Water Samples Using Liquid Chroma-tography with Electrospray Ionization Mass Spectrometric Detection

Eri Ayano, Hideko Kanazawa, Masanori Ando and Tetsuji Nishimura

Division of Environmental Chemistry, National Institute of Health Sciences, 1-18-1 Kamiyoga, Setagaya-ku, Tokyo 158-8501, Japan; Kyoritsu College of Pharmacy, 1-5-30 Shibakoen, Minato-ku, Tokyo 105-8512, Japan

Analytica Chimica Acta, Volume 507, Issue 2, 8 April 2004, Pages 211-218

Predicting Herbicides Concentrations in Paddy Water and Runoff to the River Basin

Sultana Parveen, Testuyuki Koh-guchi, Moloy Biswas, Nobukazu Nakagoshi

Graduate School for International Development and Cooperation (IDEC), Hiroshima University, Kagamiyama 1-5-1, Higashi Hiroshima 739-8529, Japan; Hiroshima Prefecture Agriculture Research Center, Hara, Hachihon-matu, Higashi Hiroshima 739-0151, Japan; Department of Environmental Studies, IDEC, Hiroshima University, Higashi Hiroshima, Japan 739-852

Journal of Environmental Sci-ences, Issue Volume 17, Number 4/2005, Pages 631-636

New Hydrophilic Materials for Solid-phase Extraction

N. Fontanals, R.M. Marcé and F. Borrull

Departament de Química Analítica i Química Orgánica, Universitat Rovira i Virgili, Campus Sescelades, Marcel·lí Domingo, s/n, E-43007 Tarragona, Spain

TrAC Trends in Analytical Chem-istry, Volume 24, Issue 5, May 2005, Pages 394-406

oASiS CArTridgESTitle Author(s) Institution(s) Journal Citation

Sulphonamide Residues in Italian Surface and Drinking Waters: A Small Scale Reconnaissance

D. Perret, A. Gentili, S. Marchese, A. Greco and R. Curini

Laboratorio Chimico per la Sicurezza, Dipartimento di Chimica, Università ``La Sapienza'', Piazzale Aldo Moro 5, P.O. Box 34, Posta 62, 00185 Roma, Italy

Chromatographia, Issue Volume 63, Numbers 5-6 / March, 2006, Pages 225-232

Occurrence of Sulfonamide Antimi-crobials in Private Water Wells in Washington County, Idaho, USA

Angela L. Batt, Daniel D. Snow and Diana S. Aga

Chemistry Department, 611 Natural Sciences Complex, University at Buffalo, The State University of New York, Buffalo, NY 14260, United States; Water Sciences Laboratory, 103 Natural Resources Hall, University of Nebraska, Lincoln, NE 68583, United States

Chemosphere Volume 64, Issue 11, September 2006, Pages 1963-1971

Multi-residue Analysis of Pharmaceu-ticals in Wastewater by Ultra-performance Liquid Chromatography–quadrupole–time-of-flight Mass Spectrometry

Mira Petrovic, Meritxell Gros and Damia Barcelo

Catalan Institution for Research and Advanced Studies (ICREA), Passeig Lluis Companys 23, 08010 Barcelona, Spain; IIQAB-CSIC, Department of Environ-mental Chemistry, Jordi Girona 18-26, 08034 Barcelona, Spain

Journal of Chromatography A Volume 1124, Issues 1-2, 18 August 2006, Pages 68-81

Determination of Sulfonamides in Selected Malaysian Swine Wastewater by High-performance Liquid Chroma-tography

Nancy T. Malintan and Mustafa Ali Mohd

Department of Pharmacology, Faculty of Medicine, University of Malaya, 50603 Kuala Lumpur, Malaysia


Determination of Several Pesticides in Water by Solid-phase Extraction, Liq-uid Chromatography and Electrospray Tandem Mass Spectrometry

Alexandre Mourão Rodrigues, Vera Ferreira, Vitor Vale Cardoso, Elisabete Ferreira and Maria João Benoliel

Laboratório Central da EPAL, Rua do Alviela 12, 1170-012 Lisbon, Portugal; Faculdade de Ciências da Universidade de Lisboa, Campo Grande Ed. C8-3°piso, 1749-016 Lisbon, Portugal


Solid-phase Extraction Combined with High-performance Liquid Chromatog-raphy Atmospheric Pressure Chemical Ionization Mass Spectrometry Analy-sis of Pesticides in Water: Method Performance and Application in a Reconnaissance Survey of Residues in Drinking Water in Greater Cairo, Egypt

Thomas L. Potter, Mahmoud A. Mohamed, and Hannah Ali

Southeast Watershed Research Laboratory, Agricultural Research Service, U.S. Department of Agriculture, Box 748, Tifton, Georgia 31793, and Department Agricultural Biochemistry, Cairo University, P.O. Box 12613, Giza 12613, Egypt

J. Agric. Food Chem., 2007, 55 (2), Pages 204–210



6 4

Liquid Chromatographic–diode-array Detection Multiresidue Determination of Rice Herbicides in Drinking and Paddy-field Water

Rafael Roehrs, Renato Zanella, Ionara Pizzuti, Martha B. Adaime, Lucía Pareja, Silvina Niell, María V. Cesio, Horacio Heinzen

Journal of AOAC International, Volume 92 | Issue: 4, Cover date: July 2009, Pages 1190-1195

Neutral Chloroacetamide Herbicide Degradates and Related Compounds in Midwestern United States Drinking Water Sources

Michelle L. Hladik, Edward J. Bouwer and A. Lynn Roberts

Department of Geography and Environmental Engineering, Johns Hopkins University, 313 Ames Hall, 3400 N. Charles St., Baltimore, MD 21218-2686, USA

Science of The Total Environment Volume 390, Issue 1, 1 February 2008, Pages 155-165

A Novel Approach for Monitoring of Cyanobacterial Toxins: Development and Evaluation of the Passive Sampler for Microcystins

Jiří Kohoutek, Pavel Babica, Luděk Bláha and Blahoslav Maršálek

Centre for Cyanobacteria and Their Toxins, Institute of Botany, The Academy of Sciences of the Czech Republic & RECETOX, Masaryk University, Kamenice 126/3, 62500 Brno, Czech Republic

Analytical and Bioanalytical Chemistry, Issue Volume 390, Number 4 / February, 2008, Pages 1167-1172

An Ultra-performance Liquid Chromatography–tandem Mass Spec-trometry Method for Determination of Microcystins Occurrence in Surface Water in Zhejiang Province, China

Jing Wang, Xiaolu Pang, Fei Ge and Zhanyu Ma

Zhejiang Province Environmental Monitoring Centre, Hangzhou, Zhejiang 310012, China; Department of Environmental Engineering, Xiangtan Univer-sity, Xiangtan, Hunan 411105, China

Toxicon Volume 49, Issue 8, 15 June 2007, Pages 1120-1128

High Performance Liquid Chromatog-raphy–tandem Mass Spectrometry for the Analysis of 10 Pesticides in Water: A Comparison Between Membrane-assisted Solvent Extraction and Solid-phase Extraction

Manuela van Pinxteren (née Schellin), Coretta Bauer and Peter Popp

Department of Analytical Chemistry, Helmholtz Centre for Environmental Research - UFZ, Permoserstrasse 15, 04318 Leipzig, Germany

Journal of Chromatography A Volume 1216, Issue 31, 31 July 2009, Pages 5800-5806

Perfluorooctane Surfactants in Waste Waters, the Major Source of River Pollution

Anna Maria Becker, Silke Gerst-mann and Hartmut Frank

Environmental Chemistry and Ecotoxicology, University of Bayreuth, D-95440 Bayreuth, Germany

Chemosphere Volume 72, Issue 1, May 2008, Pages 115-121

Multi-residue Analytical Method for the Determination of Emerging Pollutants in Water by Solid-phase Ex-traction and Liquid Chromatography–Tandem Mass Spectrometry

Rosario Rodil, José Benito Quin-tana, Purificación López-Mahía, Soledad Muniategui-Lorenzo and Darío Prada-Rodríguez

Department of Analytical Chemistry, Faculty of Sciences, University of A Coruña, Campus A Zapateira S.N., 15071 A Coruña, Spain; Department of Analytical Chemistry, Nutrition and Food Sciences, IIAA-Institute for Food Anal-ysis and Research, University of Santiago de Compostela, 15782 Santiago de Compostela, Spain; IUMA-University Institute of Environment, University of A Coruña, Pazo da Lóngora, Liáns, 15179 Oleiros (A Coruña), Spain

Journal of Chromatography A Volume 1216, Issue 14, 3 April 2009, Pages 2958-2969

Determination of Acidic Pharmaceuti-cals and Potential Endocrine Disrupt-ing Compounds in Wastewaters and Spring Waters by Selective Elution and Analysis by Gas Chromatography–mass Spectrometry

Richard Gibson, Elías Becerril-Bravo, Vanessa Silva-Castro and Blanca Jiménez

Instituto de Geografía, Universidad Nacional Autónoma de México, Ciudad Universitaria, 04510 México, D.F., Mexico; Instituto de Ingeniería, Universidad Nacional Autónoma de México, Ciudad Universitaria, 04510 México, D.F., Mexico

Journal of Chromatography A Volume 1169, Issues 1-2, 26 October 2007, Pages 31-39

Highly Sensitive Simultaneous Deter-mination of Sulfonamide Antibiotics and One Metabolite in Environmental Waters by Liquid Chromatography–Quadrupole Linear Ion Trap–mass Spectrometry

M. Silvia Díaz-Cruz, M. Jesús García-Galán and Damià Barceló

Department of Environmental Chemistry, Instituto de Investigaciones Químicas y Ambientales (IIQAB), Consejo Superior de Investigaciones Científicas (CSIC), c/Jordi Girona 18-26, E-08034 Barcelona, Spain

Journal of Chromatography A Volume 1193, Issues 1-2, 6 June 2008, Pages 50-59

Analysis of Trace Levels of Sulfon-amides in Surface Water and Soil Samples by Liquid Chromatography-Fluorescence

J. Raich-Montiu, J. Folch, R. Compañó, M. Granados and M.D. Prat

Departament de Química Analítica, Universitat de Barcelona, Martí i Franquès 1, 08028 Barcelona, Spain

Journal of Chromatography A Vol-ume 1172, Issue 2, 23 November 2007, Pages 186-193

Simplified Method for Determination of Polycarbamate Fungicide in Water Samples by Liquid Chromatography with Tandem Mass Spectrometry Fol-lowing Derivatization with Dimethyl Sulfate

Tadashi Hayama, Kunihiro Yada, Suzuko Onimaru, Hideyuki Yoshida, Kenichiro Todoroki, Hitoshi Nohta and Masatoshi Yamaguchi

Environmental Science Center, Foundation for Kyushu Environmental and Occu-pational Health, 6-4-23 Higashi-aikawa, Kurume, Fukuoka 839-0809, Japan; Faculty of Pharmaceutical Sciences, Fukuoka University, 8-19-1 Nanakuma, Johnan, Fukuoka 814-0180, Japan

Journal of Chromatography A Volume 1141, Issue 2, 9 Febru-ary 2007, Pages 251-258

Highly Sensitive Simultaneous Deter-mination of Sulfonamide Antibiotics and One Metabolite in Environmental Waters by Liquid Chromatography–Quadrupole Linear Ion Trap–mass Spectrometry

M. Silvia Díaz-Cruz, M. Jesús García-Galán and Damià Barceló

Department of Environmental Chemistry, Instituto de Investigaciones Químicas y Ambientales (IIQAB), Consejo Superior de Investigaciones Científicas (CSIC), c/Jordi Girona 18-26, E-08034 Barcelona, Spain

Journal of Chromatography A Volume 1193, Issues 1-2, 6 June 2008, Pages 50-59



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Analysis of Trace Levels of Sulfon-amides in Surface Water and Soil Samples by Liquid Chromatography-Fluorescence

J. Raich-Montiu, J. Folch, R. Compañó, M. Granados and M.D. Prat

Departament de Química Analítica, Universitat de Barcelona, Martí i Franquès 1, 08028 Barcelona, Spain

Journal of Chromatography A Vol-ume 1172, Issue 2, 23 November 2007, Pages 186-193

Simplified Method for Determination of Polycarbamate Fungicide in Water Samples by Liquid Chromatography with Tandem Mass Spectrometry Fol-lowing Derivatization with Dimethyl Sulfate

Tadashi Hayama, Kunihiro Yada, Suzuko Onimaru, Hideyuki Yoshida, Kenichiro Todoroki, Hitoshi Nohta and Masatoshi Yamaguchi

Environmental Science Center, Foundation for Kyushu Environmental and Occu-pational Health, 6-4-23 Higashi-aikawa, Kurume, Fukuoka 839-0809, Japan; Faculty of Pharmaceutical Sciences, Fukuoka University, 8-19-1 Nanakuma, Johnan, Fukuoka 814-0180, Japan


Determination of Chlorinated Acid Herbicides in Vegetation and Soil by Liquid Chromatography/Electrospray-Tandem Mass Spectrometry

Angela Schaner, Jaclyn Konecny, Laura Luckey, Heidi Hickes

Montana Department of Agriculture, Montana State University, McCall Hall, Bozeman, MT 59717

Journal of AOAC International Volume 90, Issue 5, September 2007 Pages 1402-1410

The Occurrence of Selected Antibiotics in Hong Kong Coastal Waters

A. Gulkowska, Yuhe He, M.K. So, Leo W.Y. Yeung, H.W. Leung, J.P. Giesy, Paul K.S. Lam, Michael Martin and Bruce J. Richardson

Centre for Coastal Pollution and Conservation, Department of Biology and Chemistry, City University of Hong Kong, 83 Tat Chee Avenue, Kowloon, Hong Kong SAR, People’s Republic of China; Department of Veterinary Biomedical Sciences and Toxicology Centre, University of Saskatchewan, Canada

Marine Pollution Bulletin Volume 54, Issue 8, August 2007, Pages 1287-1293

Perfluorinated Compounds in the Pearl River and Yangtze River of China

M.K. So, Y. Miyake, W.Y. Yeung, Y.M. Ho, S. Taniyasu, P. Rost-kowski, N. Yamashita, B.S. Zhou, X.J. Shi, J.X. Wang, J.P. Giesy, H. Yu and P.K.S. Lam

Centre for Coastal Pollution and Conservation, Department of Biology and Chemistry, City University of Hong Kong, Tat Chee Avenue, Kowloon, Hong Kong SAR, People’s Republic of China; National Institute of Advanced Industrial Science and Technology (AIST), 16-1 Onogawa, Tsukuba, Ibaraki 305-8569, Japan; Department of Environmental Chemistry and Ecotoxicology, University of Gdansk, Gdansk, Sobieskiego 18, Poland; State key Laboratory of Freshwater Ecology and Biotechnology, Institute of Hydrobiology, Chinese Academy of Sci-ences, Wuhan 430072, People’s Republic of China; Department of Veterinary Biomedical Sciences and Toxicology Centre, University of Saskatchewan, Canada; Zoology Department, National Food Safety and Toxicology Center, Cen-ter for Integrative Toxicology, Michigan State University, E. Lansing, MI 48823, United States; State Key Laboratory of Pollution Control and Resources, School of the Environment, Nanjing University, Nanjing 210093, People’s Republic of China

Chemosphere Volume 68, Issue 11, August 2007, Pages 2085-2095

Trace Determination of β-Lactam Antibiotics in Environmental Aque-ous Samples Using Off-line and On-line Preconcentration in Capillary Electrophoresis

M.I. Bailón-Pérez, A.M. García-Campaña, C. Cruces-Blanco and M. del Olmo Iruela

Department of Analytical Chemistry, Faculty of Sciences, Campus Fuentenueva, s/n, E-18071 Granada, Spain


Optimisation of the Separation of Herbicides by Linear Gradient High Performance Liquid Chromatography Utilising Artificial Neural Networks

Anh T.K. Tran, Ross V. Hyne, Fleur Pablo, W. Roy Day and P. Doble

Department of Chemistry, Materials and Forensic Science, Centre for Ecotoxicol-ogy, University of Technology Sydney, P.O. Box 123, Broadway, NSW 2007, Australia; Department of Environment and Conservation (NSW), Centre for Ecotoxicology, P.O. Box 29, Lidcombe, NSW 1825, Australia

Talanta Volume 71, Issue 3, 28 February 2007, Pages 1268-1275

Using Liquid Chromatography–ion Trap Mass Spectrometry to Determine Pharmaceutical Residues in Taiwanese Rivers and Wastewaters

Hsin-Chang Chen, Pi-Lien Wang and Wang-Hsien Ding

Department of Chemistry, National Central University, Chung-Li 32054, Taiwan Chemosphere Volume 72, Issue 6, June 2008, Pages 863-869

Determination of Fluoroquinolone Antibiotics in Hospital and Municipal Wastewaters in Coimbra by Liquid Chromatography with A Monolithic Column and Fluorescence Detection

M. Seifrtová, A. Pena, C. M. Lino and P. Solich

Department of Analytical Chemistry, Faculty of Pharmacy, Charles University, Heyrovského 1203, 500 05 Hradec Králové, Czech Republic; Group of Bromatology, Center of Pharmaceutical Studies, University of Coimbra, 3000 Coimbra, Portugal

Analytical and Bioanalytical Chemistry, Issue Volume 391, Number 3 / June, 2008, Pages 799-805

LC-MS-MS Analysis and Occurrence of Octyl- and Nonylphenol, Their Ethoxylates and Their Carboxylates in Belgian and Italian Textile Industry, Waste Water Treatment Plant Effluents and Surface Waters

Robert Loos, Georg Hanke, Gunther Umlauf and Steven J. Eisenreich

European Commission—DG Joint Research Centre, Institute for Environ-ment and Sustainability (IES), TP 290, Enrico Fermi, 21020 Ispra, VA, Italy; European Commission—DG Joint Research Centre, European Chemicals Bureau (ECB), Institute for Health and Consumer Protection (IHCP), TP 582, Italy

Chemosphere Volume 66, Issue 4, January 2007, Pages 690-699



66

Pharmaceutical Contamination in Residential, Industrial, and Agricul-tural Waste Streams: Risk to Aqueous Environments in Taiwan

Angela Yu-Chen Lin, Tsung-Hsien Yu and Cheng-Fang Lin

National Taiwan University, Graduate Institute of Environmental Engineering, No. 1, Section 4, Roosevelt Road, Taipei 10617, Taiwan

Chemosphere Volume 74, Issue 1, December 2008, Pages 131-141

Trace Determination of Cannabinoids and Opiates in Wastewater and Surface Waters by Ultra-performance Liquid Chromatography–tandem Mass Spectrometry

M. Rosa Boleda, M. Teresa Galceran and Francesc Ventura

AGBAR, Aigües de Barcelona, Avinguda Diagonal 211, 08018 Barcelona, Spain; University of Barcelona, Department of Analytical Chemistry, Avinguda Diagonal 647, 08028 Barcelona, Spain

Journal of Chromatography A Vol-ume 1175, Issue 1, 14 December 2007, Pages 38-48

Determination of N-methylcarbamate Pesticides in Water and Vegetable Samples by HPLC with Post-column Chemiluminescence Detection Using the Luminol Reaction

José Fernando Huertas-Pérez and Ana María García-Campaña

Department of Analytical Chemistry, Faculty of Sciences, Campus Fuentenueva, University of Granada, E-18071 Granada, Spain

Analytica Chimica Acta Volume 630, Issue 2, 23 December 2008, Pages 194-204

Determination of Commonly Used Polar Herbicides in Agricultural Drain-age Waters in Australia by HPLC

Anh T.K. Tran, Ross V. Hyne and Philip Doble

Department of Chemistry, Materials and Forensic Science, University of Tech-nology Sydney, P.O. Box 123, Broadway, NSW 2007, Australia; Department of Environmental Sciences, University of Technology Sydney, P.O. Box 123, Broadway, NSW 2007, Australia; Department of Environment and Conservation (NSW), Centre for Ecotoxicology, P.O. Box 29, Lidcombe, NSW 1825, Australia

Chemosphere Volume 67, Issue 5, March 2007, Pages 944-953

Occurrence of Psychoactive Stimula-tory Drugs in Wastewaters in North-Eastern Spain

Maria Huerta-Fontela, Maria Teresa Galceran, Jordi Martin-Alonso and Francesc Ventura

AGBAR-Aigües de Barcelona, Avinguda Diagonal 211, 08018 Barcelona, Spain; Department of Analytical Chemistry, University of Barcelona, Avinguda Diagonal 647, 08028 Barcelona, Spain

Science of The Total Environment Volume 397, Issues 1-3, 1 July 2008, Pages 31-40

An Assessment of Estrogenic Organic Contaminants in Canadian Wastewaters

Marc P. Fernandez, Michael G. Ikonomou and Ian Buchanan

University of Alberta, Department of Civil and Environmental Engineering, Edmonton, AB, Canada; Fisheries and Oceans Canada, Institute of Ocean Sci-ences, Sidney, BC, Canada

Science of The Total Environment Volume 373, Issue 1, 1 February 2007, Pages 250-269

Fate of Pharmaceuticals and Cosmetic Ingredients During the Operation of A MBR Treating Sewage

R. Reif, S. Suárez, F. Omil and J.M. Lema

Department of Chemical Engineering, School of Engineering, University of Santiago de Compostela, Avda. Lope Gómez de Marzoa s/n, E-15782, Santiago de Compostela, Spain

Desalination Volume 221, Issues 1-3, 1 March 2008, Pages 511-517

Organochlorinated Pesticide Multi-residues in Surface Sediments from Beijing Guanting Reservoir

Nandong Xue, Daren Zhang and Xiaobai Xu

Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, State Key Laboratory of Environmental Chemistry and Ecotoxicology, 18 Shuangqing Road, Beijing 100085, China

Water Research Volume 40, Issue 2, January 2006, Pages 183-194

Spatial and Temporal Analysis of Pharmaceutical Concentrations in the Upper Tennessee River Basin

Justin M. Conley, Steven J. Symes, Mark S. Schorr and Sean M. Richards

Department of Biological and Environmental Sciences, University of Tennessee at Chattanooga, 615 McCallie Avenue, Chattanooga, TN 37403, United States; Department of Chemistry, University of Tennessee at Chattanooga, United States

Chemosphere Volume 73, Issue 8, November 2008, Pages 1178-1187

Fast Determination of Herbicides in Waters by Ultra-performance Liquid Chromatography/Tandem Mass Spectrometry

Elena Pastor Montoro, Roberto Romero González, Antonia Gar-rido Frenich, M. Elena Hernández Torres, Jose Luis Martínez Vidal

Laboratory of Pesticide Residues LAB, Avda. del Mediterráneo, S/N, Edif. Calablanca Bajo 04009 Almería, Spain; Group Analytical Chemistry of Contaminants, Department of Analytical Chemistry, University of Almería, E-04071 Almería, Spain

Rapid Communications in Mass Spectrometry Volume 21 Issue 22, Pages 3585 - 3592

Occurrence and Fate of Antibiotics in the Seine River in Various Hydrologi-cal Conditions

Fatima Tamtam, Fabien Mercier, Barbara Le Bot, Joëlle Eurin, Quoc Tuc Dinh, Michel Clément and Marc Chevreuil

Université Pierre et Marie Curie/ EPHE, UMR Sisyphe 7619, 4 place Jussieu, BC 105, 75252 Paris Cedex, France; Ecole Nationale de la Santé Publique, Laboratoire d'Etude et de Recherche en Environnement et Santé (LERES), Av-enue Professeur Léon Bernard, 35000 Rennes, France; Laboratoire Hydrologie et Environnement, EPHE , UMR Sisyphe 7619, Université Pierre et Marie Curie, 4 place Jussieu, BC 105, 75252 Paris Cedex, France

Science of The Total Environment Volume 393, Issue 1, 1 April 2008, Pages 84-95

Pharmaceutical Compounds in the Wastewater Process Stream in Northwest Ohio

Alison L. Spongberg and Jason D. Witter

Department of Environmental Sciences, Mail Stop 604, University of Toledo, Toledo, Ohio 43606, USA

Science of The Total Environment Volume 397, Issues 1-3, 1 July 2008, Pages 148-157

Analysis of Pharmaceuticals in Wastewater and Removal Using A Membrane Bioreactor

Jelena Radjenovic, Mira Petrovic and Damiá Barceló

Department of Environmental Chemistry, IIQAB-CSIC, C/Jordi Girona 18-26, 08034 Barcelona, Spain; Institucio Catalana de Reserca i Estudis Avanzats (ICREA), 08010 Barcelona, Spain

Analytical and Bioanalytical Chemistry, Issue Volume 387, Number 4 / February, 2007, Pages 1365-1377



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Impact of Pesticides Used in Agricul-ture and Vineyards to Surface and Groundwater Quality (North Spain)

Alain Hildebrandt, Míriam Guillamón, Sílvia Lacorte, Romà Tauler and Damià Barceló

Department of Environmental Chemistry, IIQAB-CSIC, Jordi Girona 18-26, 08034 Barcelona, Catalonia, Spain

Water Research Volume 42, Issue 13, July 2008, Pages 3315-3326

Recent Advances in LC-MS Residue Analysis of Veterinary Medicines in the Terrestrial Environment

M. Silvia Díaz-Cruz and Damià Barceló

Department of Environmental Chemistry, IIQAB-CSIC, University of Barcelona, C/Jordi Girona 18-26, Barcelona E-08034, Spain

TrAC Trends in Analytical Chem-istry Volume 26, Issue 6, June 2007, Pages 637-646

Identification and Quantification of Ibuprofen, Naproxen, Ketoprofen and Diclofenac Present in Waste-waters, as Their Trimethylsilyl Derivatives, by Gas Chromatography Mass Spectrometry

Á. Sebők, A. Vasanits-Zsigrai, Gy. Palkó, Gy. Záray and I. Molnár-Perl

Institute of Chemistry, Department of Analytical Chemistry, L. Eötvös Universi-ty, Hungary; Cooperative Research Center of Environmental Sciences, H-1518, Budapest 112, P.O. Box 32, Hungary; Budapest Sewage Works Limited, 1087 Budapest, Asztalos Sándor Street 4, Hungary

Talanta Volume 76, Issue 3, 30 July 2008, Pages 642-650 "

ACQuiTy ColuMNSTitle Author(s) Institution(s) Journal Citation

Ultra Trace Determination of 31 Pesticides in Water Samples by Direct Injection–rapid Resolution Liquid Chromatography-electrospray Tandem Mass Spectrometry

Laura Díaz, Julio Llorca-Pórcel and Ignacio Valor

LABAQUA S.A. C/Dracma 16-18, Polígono industrial las Atalayas, 03114 Alicante, Spain

Analytica Chimica Acta Volume 624, Issue 1, 22 August 2008, Pages 90-96

Challenges and Achievements of LC-MS in Environmental Analysis: Twenty-five years On

Damia Barceló and Mira Petrovic Department of Environmental Chemistry, IIQAB-CSIC, Jordi Girona, 18–26, 08034 Barcelona, Spain

TrAC Trends in Analytical Chem-istry Volume 67, Issue 5, March 2007, Pages 944-953

Comparison of Matrix Effects in HPLC-MS/MS and UPLC-MS/MS Analysis of Nine Basic Pharmaceuticals in Surface Waters

Jet C. Van De Steene and Willy E. Lambert

Laboratory of Toxicology, Ghent University, Ghent, Belgium Journal of the American Society for Mass Spectrometry Volume 19, Issue 5, May 2008, Pages 713-718

Determination of Ofloxacin Enantiom-ers in Sewage Using Two-step Solid-phase Extraction and Liquid Chromatography with Fluorescence Detection

Bing Shao, Xiaojie Sun, Jing Zhang, Jianying Hu, Huiru Dong and Yi Yang

Beijing Center for Disease Control and Prevention, Beijing 100013, China; College of Urban and Environmental Science, Peking University, Beijing 100871, China; Beijing University of Chemical Technology, Beijing 100029, China; School of Public Health and Family Medicine, Capital Medical University, Beijing 100089, China


Determination of Polycyclic Aromatic Hydrocarbons in Soil by Ultra Perfor-mance Liquid Chromatography

Chen H, Liu Y, Liu H, Yuan Y, Xiao Q

State Key Laboratory of Pollution Control and Resource Reuse, College of Environmental Science and Engineering, Tongji University, Shanghai 200092, China

Se Pu. 2008 Nov;26(6):769-71.

Analysis of Perfluorinated Carboxylic Acids in Soils II: Optimization of Chro-matography and Extraction

John W. Washington, W. Matthew Henderson, J. Jackson Ellington, Thomas M. Jenkins and John J. Evans

United States Environmental Protection Agency, National Exposure Research Laboratory, 960 College Station Road, Athens, GA 30605, USA; Senior Service America Inc., United States Environmental Protection Agency, National Exposure Research Laboratory, 960 College Station Road, Athens, GA 30605, USA

Journal of Chromatography A Volume 1181, Issues 1-2, 15 February 2008, Pages 21-32

XBridgE ColuMNSTitle Author(s) Institution(s) Journal Citation

Analysis of Lagoon Samples from Dif-ferent Concentrated Animal Feeding Operations for Estrogens and Estrogen Conjugates

Stephen R. Hutchins, Mark V. White, Felisa M. Hudson, and Dennis D. Fine

Ground Water and Ecosystems Restoration Division, National Risk Management Research Laboratory, U.S. Environmental Protection Agency, P.O. Box 1198, Ada, Oklahoma 74821-1198, and Shaw Environmental and Infrastructure, P.O. Box 1198, Ada, Oklahoma 74821-1198, USA

Environ. Sci. Technol., 2007, 41 (3), Pages 738–744

25,000-fold Pre-concentration in A Single Step with Liquid-phase Microextraction

Tung Si Ho, Terje Vasskog, Trude Anderssen, Einar Jensen, Knut Einar Rasmussen and Stig Pedersen-Bjergaard

School of Pharmacy, University of Oslo, Oslo, Norway; bInstitute for Pharmacy, University of Tromsø, Tromsø, Norway

Analytica Chimica Acta Volume 592, Issue 1, 29 May 2007, Pages 1-8



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Occurrence of Selective Serotonin Reuptake Inhibitors in Sewage and Receiving Waters at Spitsbergen and in Norway

Terje Vasskog, Trude Anderssen, Stig Pedersen-Bjergaard, Roland Kallenborn and Einar Jensen

Department of Pharmacy, Faculty of Medicine, University of Tromsø, Tromsø, Norway; School of Pharmacy, University of Oslo, Oslo, Norway; The University Centre in Svalbard, Longyearbyen, Norway


Ultratrace-level Determination of Glyphosate, Aminomethylphosphonic Acid and Glufosinate in Natural Waters by Solid-phase Extraction Followed by Liquid Chromatography–tandem Mass Spectrometry: Performance Tuning of Derivatization, Enrichment and Detection

Irene Hanke, Heinz Singe and Juliane Hollender

Eawag, Environmental Chemistry, Ueberlandstrasse 133, 8600 Duebendorf, Switzerland

Analytical and Bioanalytical Chemistry; Issue Volume 391, Number 6 / July, 2008; Pages 2265-2276

Comprehensive Liquid Chromatogra-phy-ion-spray Tandem Mass Spectrom-etry Method for the Identification and Quantification of Eight Hydroxylated Brominated Diphenyl Ethers in Envi-ronmental Matrices

Sílvia Mas, Olga Jáuregui, Fernando Rubio, Anna de Juan, Romà Taule, Sílvia Lacorte

Department of Environmental Chemistry, IIQAB-CSIC, Jordi Girona 18-26, 08034 Barcelona, Catalonia, Spain; Scientific and Technical Services, University of Barcelona, Josep Samitier 1-5, 08028 Barcelona, Catalonia, Spain; ABRAXIS LLC, Northampton Business Center, 54 Steamwhistle Drive, Warminster, Pennsylvania 18974, USA; Department of Analytical Chemistry, University of Barcelona, Diagonal 647, 08028 Barcelona, Catalonia, Spain

Journal of Mass Spectrometry Vol-ume 42 Issue 7, Pages 890 - 899

Comparing Solid-phase Extraction and Direct Injection for the Analysis of Ul-tra-trace Levels of Relevant Explosives in Lake Water and Tributaries Using Liquid Chromatography–electrospray Tandem Mass Spectrometry

Ueli Ochsenbein, Markus Zeh and Jean-Daniel Berset

Water and Soil Protection Laboratory (WSPL), Department of Organic Analytical Chemistry, Schermenweg 11, 3014 Bern, Switzerland

Chemosphere Volume 72, Issue 6, June 2008, Pages 974-980

SuNfirE ColuMNSTitle Author(s) Institution(s) Journal Citation

Quantitative Determination of Three Sulfonamides in Environmental Water Samples Using Liquid Chromatography Coupled to Electrospray Tandem Mass Spectrometry

Doreen Richter, Uwe Dünnbier, Gudrun Massmann Asaf Pekdeger

Institute of Geological Sciences, Freie Universität Berlin, Malteserstr. 74-100, 12249 Berlin, Germany; Department of Laboratories, Berlin Water Company, 10864 Berlin, Germany

Journal of Chromatography A Volume 1157, Issues 1-2, 20 July 2007, Pages 115-121

On-line Solid-phase Extraction with On-support Derivatization for High-sensitivity Liquid Chromatog-raphy Tandem Mass Spectrometry of Estrogens in Influent/Effluent of Wastewater Treatment Plants

Arnaud Salvador, Cedric Moret-ton, Anne Piram and René Faure

Université Claude Bernard Lyon 1, UMR 5180, 43 Boulevard du 11 novembre 1918, 69622 Villeurbanne cedex, France

Journal of Chromatography A Volume 1145, Issues 1-2, 23 March 2007, Pages 102-109

Determination of Low-level Pesticide Residues in Soft Drinks and Sports Drinks by Liquid Chromatography with Tandem Mass Spectrometry: Collaborative Study

Kathleen D. Miller and Paul Milne Covance Laboratories, 3301 Kinsman Blvd, Madison, WI 53704; PepsiCo Inc., 100 Stevens Ave, Valhalla, NY 10595.

Journal of AOAC INTERNATIONAL Volume: 91 | Issue: 1 Cover date: January 2008 Page(s): 181-201

Seasonal and Diurnal Fluctuations in the Concentrations of Pharmaceuticals and Personal Care Products (PPCPs) in Residential Sewage Water

Yuji Takao, Miki Shimazu, Mayumi Fukuda, Hiroshi Ishibashi, Masaki Nagae, Shinya Kohra, Yasuhiro Tabira, Yasuhiro Ishibashi and Koji Arizono

Faculty of Environmental Studies, Nagasaki University; Faculty of Environmen-tal and Symbiotic Sciences, Prefectural University of Kumamoto; Joint Research Center, Nagasaki University; Faculty of Human Environment, Nagasaki Institute of Applied Science

J. Health Sci., Volume 54, Pages 240-243 (2008)

Determination of Seven Polyphenols in Water by High Performance Liquid Chromatography Combined with Preconcentration

Qian Liu, Wensheng Cai and Xueguang Shao

Research Center for Analytical Sciences, College of Chemistry, Nankai Univer-sity, Weijin Road No. 94, Tianjin 300071, PR China

Talanta Volume 77, Issue 2, 15 December 2008, Pages 679-683

Abscisic Acid and Drought Response of Canarian Laurel Forest Tree Species Growing Under Controlled Conditions

Manuel Sánchez-Díaz, Carolina Tapia and M. Carmen Antolín

Departamento de Biología Vegetal, Facultades de Ciencias y Farmacia, Universi-dad de Navarra, Irunlarrea s/n, 31008 Pamplona, Spain

Environmental and Experimental Botany Volume 64, Issue 2, No-vember 2008, Pages 155-161

Glufosinate and Ammonium Sulfate Inhibit Atrazine Degradation in Adapted Soils

Robert M. Zablotowicz, L. Jason Krutz, Mark A. Weaver, Cesare Accinelli and Krishna N. Reddy

USDA-ARS, Southern Weed Science Research Unit, Stoneville, MS, USA; Dept. of Agro-Environmental Science & Technology, University of Bologna, Bologna, Italy

Biology and Fertility of Soils, Issue Volume 45, Number 1 / October, 2008, Pages 19-26



69

Ergot Alkaloids in Norwegian Wild Grasses: A Mass Spectrometric Approach

Silvio Uhlig, Turid Vikøren, Lada Ivanova, Kjell Handeland

National Veterinary Institute, P.O. Box 8156 Dep., 0033 Oslo, Norway Rapid Communications in Mass Spectrometry Volume 21 Issue 10, Pages 1651-1660

ATlANTiS ColuMNSTitle Author(s) Institution(s) Journal Citation

Evaluation of A Multiresidue Method for Measuring Fourteen Chemical Groups of Pesticides in Water by Use of LC-MS-MS

J. J. Carvalho, P. C. A. Jerónimo, C. Gonçalves and M. F. Alpen-durada

IAREN-Water Institute of the Northern Region, Rua Dr. Eduardo Torres, 229, 4450–113 Matosinhos, Portugal; FFUP-Faculty of Pharmacy, University of Porto, Laboratory of Hydrology, Rua Aníbal Cunha 164, 4050–047 Porto, Portugal

Analytical and Bioanalytical Chemistry, Issue Volume 392, Number 5 / November, 2008, Pages 955-968

Source to Sink Tracking of Selected Human Pharmaceuticals from Two Oslo City Hospitals and A Wastewater Treatment Works

Kevin V. Thomas, Christian Dye, Martin Schlabach and Katherine H. Langford

J. Environ. Monit., 2007, 9, 1410-1418

Eliminating Solid Phase-extraction with Large-volume Injection LC/MS/MS: Analysis of Illicit and Legal Drugs and Human Urine Indicators in US Wastewaters

Aurea C. Chiaia, Caleb Banta-Green and Jennifer Field

Department of Chemistry and Department of Environmental Toxicology, Oregon State University, Corvallis, Oregon 97331, and Alcohol and Drug Abuse Institute, University of Washington, Seattle, Washington 98105, USA

Environ. Sci. Technol., 2008, 42 (23), Pages 8841–8848

Determination of Several Pesticides in Water by Solid-phase Extraction, Liq-uid Chromatography and Electrospray Tandem Mass Spectrometry

Alexandre Mourão Rodrigues, Vera Ferreira, Vitor Vale Cardoso, Elisabete Ferreira and Maria João Benoliel

Laboratório Central da EPAL, Rua do Alviela 12, 1170-012 Lisbon, Portugal; Faculdade de Ciências da Universidade de Lisboa, Campo Grande Ed. C8-3°piso, 1749-016 Lisbon, Portugal


Monitoring of Pesticides in Agricul-tural Water and Soil Samples from Andalusia by Liquid Chromatography Coupled to Mass Spectrometry

A. Belmonte Vega, A. Garrido Frenich and J.L. Martínez Vidal-Corresponding Author Contact Information

Department of Analytical Chemistry, University of Almería, 04071 Almería, Spain

Analytica Chimica Acta Volume 538, Issues 1-2, 4 May 2005, Pages 117-127

Residue Determination of Glyphosate, Glufosinate and Aminomethylphos-phonic Acid in Water and Soil Samples by Liquid Chromatography Coupled to Electrospray Tandem Mass Spectrometry

María Ibáñez, Óscar J. Pozo, Juan V. Sancho, Francisco J. López and Félix HernándezCorrespond-ing Author Contact Information

Research Institute for Pesticides and Water, University Jaume I, E-12071 Castellón, Spain

Journal of Chromatography A Volume 1081, Issue 2, 22 July 2005, Pages 145-155

Determination of Antimicrobials in Sludge from Infiltration Basins at Two Artificial Recharge Plants by Pressurized Liquid Extraction–liquid Chromatography–tandem Mass Spectrometry

M. Silvia Díaz-Cruzr, M José Ló-pez de Aldaaand Damià Barceló

Department of Environmental Chemistry, Instituto de Investigaciones Químicas y Ambientales (IIQAB), Consejo Superior de Investigaciones Científicas (CSIC), c/Jordi Girona 18-26, 08034 Barcelona, Spain

Journal of Chromatography A Vol-ume 1130, Issue 1, 13 October 2006, Pages 72-82

PAH ColuMNSTitle Author(s) Institution(s) Journal Citation

Development of A Matrix Solid-phase Dispersion Method for the Determina-tion of Polycyclic Aromatic Hydrocar-bons in Sewage Sludge Samples

M. Teresa Pena, M. Carmen Casais, M. Carmen Mejuto and Rafael Cela


Analytica Chimica Acta Volume 626, Issue 2, 26 September 2008, Pages 155-165

Identification of A Water Pollutant, 2-amino-6,7-dichlorobenzothiazole, at A River Near A Textile Industrial Complex in Korea

J.-H. Kwon, J.-W. Kwon, K. Kim and Y.-H. Kim

Environmental Chemistry Laboratory, Korea Research Institute of Chemical Technology, Post Office Box 107, Yusong, Taejon, 305-600, Korea, KR; National Veterinary Research and Quarantine Service Pusan Regional Office 620-2, Amnam-dong, Seo-gu, Pusan, 602-030, Korea, KR

Bulletin of Environmental Con-tamination and Toxicology, Issue Volume 70, Number 1 / January, 2003, Pages 0054-0062

Optimization of the Matrix Solid-phase Dispersion Sample Preparation Procedure for Analysis of Polycyclic Aromatic Hydrocarbons in Soils: Comparison with Microwave-assisted Extraction

M.T. Pena, M.C. Casais, M.C. Mejuto and R. Cela





70

Fungal Communities in PAH-impacted Sediments of Genoa-voltri Harbour (NW Mediterranean, Italy)

V.S. Salvo, I. Gallizia, M. Moreno and M. Fabiano

Dipartimento per lo Studio del Territorio e delle sue Risorse (DIP.TE.RIS.), Università di Genova, C. so Europa 26, Genova 16132, Italy

Marine Pollution Bulletin Volume 50, Issue 5, May 2005, Pages 553-559

Evaluation of the Genotoxicity of River Sediments from Industrialized and Unaffected Areas Using A Battery of Short-term Bioassays

Assia Aouadene, Carole Di Giorgio, Luc Sarrazin, Xavier Moreau, Laetitia De Jong, Fabrice Garcia, Alain Thiery, Alain Botta, Michel De Méo

Laboratoire de Biogénotoxicologie et Mutagenèse Environnementale, Université de la Méditerranée, Facultés de Médecine et Pharmacie, Marseille, France; Laboratoire d'Hydrologie et de Molysmologie Aquatique, Université de la Méditerranée, Faculté de Pharmacie, Marseille, France; UMR-Centre National de la Recherche Scientifique 6116 IMEP, Case 17, Université de Provence, Marseille, France

Environmental and Molecular Mutagenesis Volume 49 Issue 4, Pages 283-299

Effects of Dissolved Organic Matter from Sewage Sludge on the Atrazine Sorption by Soils

Ling Wanting, Jianming Xu and Yanzheng Gao

College of Environmental and Natural Resource Sciences, Zhejiang University, 310029 Hangzhou, China; College of Natural Resource and Environmental Sciences, Nanjing Agricultural University, 210095 Najing, China

Science in China Series C: Life Sciences, Issue Volume 48, Supplement 1 / January, 2005, Pages 57-66

CArBAMATE ColuMNSTitle Author(s) Institution(s) Journal Citation

Automated In-tube Solid-phase Microextraction–high-performance Liquid Chromatography for Carbamate Pesticide Analysis

Yanni Gou, Ralf Eisert and Janusz Pawliszyn

Guelph-Waterloo Centre for Graduate Work in Chemistry, Department of Chem-istry, University of Waterloo, Waterloo, Ontario N2L 3G1, Canada


Simultaneous Determination of Neo-nicotinoid Insecticides in Agricultural Samples by Solid-phase Extraction Cleanup and Liquid Chromatography Equipped with Diode-array Detection

Eiki Watanabe, Koji Baba, and Heesoo Eun

National Institute for Agro-Environmental Sciences, Kannondai 3-1-3, Tsukuba, Ibaraki 305-8604, Japan

J. Agric. Food Chem., 2007, 55 (10), Pages 3798–3804

Influence of Methanol on Retention of Hydrophobic Organic Chemicals in Soil Leaching Column Chroma-tography

Feng Xu, Bingcheng Lin, Fan Su, Karl-Werner Schrammband Antonius Kettrup

Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 161 Zhongshan Road, Dalian 116011, China; GSF-National Research Center for Environment and Health, Institute of Ecological Chemistry, Ingolstädter Landstrasse 1, D-85764 Neuherberg, Germany

Chemosphere Volume 48, Issue 1, July 2002, Pages 149-156

Fast Chromatography of Complex Biocide Mixtures Using Diode Array Detection and Multivariate Curve Resolution

Emma Peré-Trepat, Alain Hil-debrandt, Damià Barceló, Silvia Lacorte and Romà Tauler

Department of Analytical Chemistry, Universitat de Barcelona, Diagonal 647, 08028 Barcelona, Spain; Department of Environmental Chemistry, IIQAB-CSIC, Jordi Girona 18-26, 08034 Barcelona, Spain

Chemometrics and Intelligent Laboratory Systems Volume 74, Issue 2, 28 December 2004, Pages 293-303

Determination of N-methylcarbamate Pesticides in Water and Vegetable Samples by HPLC with Post-column Chemiluminescence Detection Using the Luminol Reaction

José Fernando Huertas-Péreza and Ana María García-Campaña-Corresponding Author Contact Information

Department of Analytical Chemistry, Faculty of Sciences, Campus Fuentenueva, University of Granada, E-18071 Granada, Spain

Analytica Chimica Acta Volume 630, Issue 2, 23 December 2008, Pages 194-204

Determination of Benzimidazole Fungicides by HPLC with Fluorescence Detection After Micellar Extraction

R. Halko, C. Padron Sanz, Z. Sosa Ferrera and J. J. Santana Rodríguez

Department of Analytical Chemistry, Faculty of Natural Sciences, Comenius University, Bratislava 842 15, Slovakia; Department of Chemistry, Faculty of Marine Sciences, University of Las Palmas de G. C., Las Palmas de G.C, 35017, Spain

Chromatographia, Issue Volume 60, Numbers 3-4 / August, 2004, Pages 151-156

Determination of Benzimidazole Fungicides in Soil Samples Using Microwave-assisted Micellar Extraction and Liquid Chromatography with Fluorescence Detection

Radoslav Halko, Carolina Padrón Sanz, Zoraida Sosa Ferrera, José Juan Santana Rodríguez

Journal of AOAC INTERNATION-AL, Volume: 89 | Issue: 5 Cover date: September/October 2006 Page(s): 1403-1409

Multiresidue Analytical Methods for the Ultra-trace Quantification of 33 Priority Substances Present in the List of Reach in Real Water Samples

Jean-Baptiste Baugros, Barbara Giroud, Guy Dessalces, Marie-Florence Grenier-Loustalot and Cécile Cren-Olivé

Service Central d’Analyse du CNRS, Vernaison, France; Service Central d’Analyse du CNRS – USR59, Echangeur de Solaize Chemin du Canal, BP 22, 69360 Solaize, France

Analytica Chimica Acta Volume 607, Issue 2, 28 January 2008, Pages 191-203

Sorption and Mobility of Ivermectin in Different Soils

K.A. Krogh, T. Søeborg, B. Brodin and B. Halling-Sørensen

Copenhagen Univ., Faculty of Pharmaceutical Science, Dep. of Pharmaceutics and Analytical Chemistry, Section of Toxicology and Environmental Chemistry, Universitetsparken 2, DK-2100 Copenhagen, Denmark

J Environ Qual 37, Pages 2202-2211 (2008)



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