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COSMOSIL PYE and NPE - Hichrom · In COSMOSIL NPE, on the other hand, isomers with a strong dipole...

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COSMOSIL PYE (pyrenylethyl group bonded) and COSMOSIL NPE (nitrophenylethyl group bonded) column show unique retention characteristics based on multiple separation modes such as hydrophobic, charge transfer and - interactions. These columns are recommended for the separation of structural isomers. COSMOSIL COSMOGEL Specialty for Structual Isomers COSMOSIL PYE / COSMOSIL NPE Separation of PAHs Due to the planar pyrene ring structure and strong - interactions, COSMOSIL PYE achieves excellent separation of aromatic isomers. Column size Mobile phase Flow rate Temperature Detection 4.6mmI.D. x 150mm Methanol:Water=90:10 1.0ml/min 30 o C UV 254nm Material characteristics Packing material Silica gel Average particle size Average pore size Specific surface area Stationary phase Main interaction End-capping treatment Carbon content COSMOSIL 5PYE 2-(1-pyrenyl)ethyl group Hydrohobic interaction - interaction Charge transfer interaction Stereo selectivity approx. 18% Sample 1. Benz [a] anthracene 2. Chrysene COSMOSIL 5NPE nitrophenylethyl group Hydrohobic interaction, - interaction Charge transfer interaction Dipole-dipole interaction approx. 9% high purity spherical porous silica 5m approx. 120 approx. 300m 2 /g near-perfect treatment Si H 3 C CH 3 Si H 3 C CH 3 NO 2 PYE NPE Column size Mobile phase Flow rate Temperature Detection Sample 4.6mmI.D. x 150mm A: Water, B: Methanol B 80% B 100% 20min. Linear gradient 1.0ml/min 30 o C UV 254nm 1. Naphthalene 2. Acenaphthylene 3. Axenaphthene 4. Flourene 5. Phenathrene 6. Anthracene 7. Fluoranthene 8. Pyrene 9. 2, 3-Benzofluorene 10. Benz [a] anthracene 11. Chrysene 12. Triphenylene 13. Naphthacene 14. Benzo[a] pyrene 15. Perylene 16. Dibenz [a,c] anthracene 17. Dibenz [a,h] anthracene 1. Benz [a] anthracene 2. Chrysene COSMOSIL 5PYE COSMOSIL 5C18-MS-II COSMOSIL 5PYE Separation of ACHs (Adrenal Cortical Hormones) Column Size Flow rate Temperature Detection COSMOSIL 5PYE 4.6mmI.D. x 150mm 1.0ml/min 30 o C UV 295nm Mobile phase: 80% Methanol Mobile phase: 40% Methanol O HO O CH 2 OH OH O HO O CH 2 OH OH 2 3 Sample 1. Phenol 2. Prednisolone 3. Hydrocortisone COSMOSIL COSMOGEL
Transcript
Page 1: COSMOSIL PYE and NPE - Hichrom · In COSMOSIL NPE, on the other hand, isomers with a strong dipole moment are retained preferentially. Both COSMOSIL PYE and NPE offer special resolutions

COSMOSIL PYE (pyrenylethyl group bonded) and COSMOSIL NPE (nitrophenylethyl group bonded) column show unique retention

characteristics based on multiple separation modes such as hydrophobic, charge transfer and - interactions. These columns

are recommended for the separation of structural isomers.

COSMOSILCOSMOGEL

Specialty for Structual Isomers

COSMOSIL PYE / COSMOSIL NPE

Separation of PAHsDue to the planar pyrene ring structure and strong - interactions, COSMOSIL PYE achieves excellent separation of

aromatic isomers.

Column size

Mobile phase

Flow rate

Temperature

Detection

4.6mmI.D. x 150mm

Methanol:Water=90:10

1.0ml/min

30oC

UV 254nm

Material characteristicsPacking material

Silica gel

Average particle size

Average pore size

Specific surface area

Stationary phase

Main interaction

End-capping treatment

Carbon content

COSMOSIL 5PYE

2-(1-pyrenyl)ethyl group

Hydrohobic interaction

- interaction

Charge transfer interaction

Stereo selectivity

approx. 18%

Sample 1. Benz [a] anthracene

2. Chrysene

COSMOSIL 5NPE

nitrophenylethyl group

Hydrohobic interaction,

- interaction

Charge transfer interaction

Dipole-dipole interaction

approx. 9%

high purity spherical porous silica

5 m

approx. 120

approx. 300m2/g

near-perfect treatment

SiH3C CH3SiH3C CH3

NO2

PYE NPE

Column size

Mobile phase

Flow rate

Temperature

Detection

Sample

4.6mmI.D. x 150mm

A: Water, B: Methanol

B 80% B 100%

20min. Linear gradient

1.0ml/min

30oC

UV 254nm

1. Naphthalene

2. Acenaphthylene

3. Axenaphthene

4. Flourene

5. Phenathrene

6. Anthracene

7. Fluoranthene

8. Pyrene

9. 2, 3-Benzofluorene

10. Benz [a] anthracene

11. Chrysene

12. Triphenylene

13. Naphthacene

14. Benzo[a] pyrene

15. Perylene

16. Dibenz [a,c] anthracene

17. Dibenz [a,h] anthracene

1. Benz [a] anthracene 2. Chrysene

COSMOSIL 5PYE COSMOSIL 5C18-MS-II COSMOSIL 5PYE

Separation of ACHs (Adrenal Cortical Hormones)

Column

Size

Flow rate

Temperature

Detection

COSMOSIL 5PYE

4.6mmI.D. x 150mm

1.0ml/min

30oC

UV 295nm

Mobile phase: 80% Methanol Mobile phase: 40% Methanol

O

HO

OCH2OH

OH

O

HO

OCH2OH

OH

2 3

Sample 1. Phenol

2. Prednisolone

3. Hydrocortisone

COSMOSIL

COSMOGEL

Page 2: COSMOSIL PYE and NPE - Hichrom · In COSMOSIL NPE, on the other hand, isomers with a strong dipole moment are retained preferentially. Both COSMOSIL PYE and NPE offer special resolutions

Effect of - interaction

COSMOSIL 5NPE COSMOSIL 5PYE

The ODS column cannot sharply separate the positional isomers like phthalonitrile. In contrast, COSMOSIL PYE and NPE

can do it very well by - interaction. Furthermore, COSMOSIL NPE strongly retains ortho compound which has a big

dipole moment.

o- p-m-

Analysis of disubstituted naphtalenes

Column size

Mobile phase

Flow rate

Temperature

Detection

Sample

4.6mmI.D. x 150mm

PYE: Methanol:Water=90:10

NPE: Methanol:Water=70:30

ODS: Methanol:Water=80:20

1.0ml/min

30oC

COSMOSIL 5PYE

COSMOSIL PYE and NPE columns show very unique retention characteristics for compounds containing electron donors

and acceptors. These substances elute according to their hydrophobicity in ODS columns. In COSMOSIL PYE and NPE,

on the other hand, dinitronaphthalenes are retained more strongly. That means charge transfer interaction contributes to

the retention of dinitronaphthalenes. Furthermore, COSMOSIL PYE retains 1,5-dinitronaphthalene (Sample 2) more

strongly than the 1,8- form (Sample 1), due to the charge transfer interaction. In the COSMOSIL NPE, on the other hand,

Sample 1 is retained more strongly. In addition to - interaction, dipole-dipole interaction is utilized for its retention.

Column size

Mobile phase

Flow rate

The chromatograms below are examples for analysis of the electron donor anisole and the electron acceptors nitroben-

zene and benzene. COSMOSIL PYE, conventional Ph and ODS show different elution orders and reteintion times.

Effect of dipole-dipole interaction

4.6mmI.D. x 150mm

NPE: Methanol:Water=40:60

PYE: Methanol:Water=80:20

ODS: Methanol:Water=30:70

1.0ml/min

Temperature

Detection

Sample

30oC

UV 254nm

1. o-Phthalonitrile

2. m-Phthalonitrile

3. p-Phthalonitrile

(0.30 g)

(3.00 g)

(0.15 g)

CN

CN

CN

CN

CN

CN

Conventional ODS

COSMOSIL 5PYE Conventional Ph

1 32

Column size

Mobile phase

Flow rate

4.6mmI.D. x 150mm

PYE: Methanol:Water=50:50

Ph: Methanol:Water=40:60

ODS: Methanol:Water=50:50

1.0ml/min

Temperature

Detection

Sample

30oC

UV 254nm

1. Nitrobenzene

2. Anisole

3. Benzene

(0.125 g)

(1.50 g)

(4.00 g)

Conventional ODS

NO2 OCH3

(0.21 g)

(0.11 g)

(0.25 g)

(0.35 g)

(0.42 g)

1. 1,8-Dinitronaphtalene

2. 1,5-Dinitronaphtalene

3. Naphtalene

4. 1-Methylnaphtalene

5. 1,5-Dimethylnaphtalene

NO2 NO2

NO2

NO2 CH3CH3

CH3

COSMOSIL 5NPE Conventional ODS

Separation of Tocopherols

COSMOSIL 5PYE COSMOSIL 5NPE Cnventional ODS

Column size

Mobile phase

Flow rate

Temperature

Detection

4.6mmI.D. x 150mm

PYE: 90% methanol

ODS: 95% methanol

1.0ml/min

30oC

UV 295nm

Sample 1. -Tocopherol

2. -Tocopherol

3. -Tocopherol

4. -Tocopherol

Conventional Ph

(min)

Conventional ODS

3

2

1

3 21

3

2

1

Page 3: COSMOSIL PYE and NPE - Hichrom · In COSMOSIL NPE, on the other hand, isomers with a strong dipole moment are retained preferentially. Both COSMOSIL PYE and NPE offer special resolutions

T

m-

p-

o-

B

Advantage of dipole-dipole interactions

The chromatogram below illustratews the separation of o-, m-, p-tolunitrile. ODS column cannot achieve complete separa-

tion of them, while COSMOSIL NPE separates them more greatly.

Comparing hydrophobicity, tolunitrile which contains a CN- group is lower in its hydrophobicity than benzene and toluene.

Since hydrophobic interaction is dominant in the separation by a ODS column, tolunitrile elutes first. In COSMOSIL NPE,

tolunitrile elutes later. This suggests that COSMOSIL NPE utilizes the interaction between -electron of the nitrophenyl

group and CN- for retention in addition to hydrophobic interaction.

COSMOSIL 5NPE Conventional ODS

Column size

Mobile phase

Flow rate

Temperature

Detection

4.6mmI.D. x 150mm

Methanol:Water=50:50

1.0ml/min

30oC

UV 295nm

CH3

CN

CH3

Tolunitrile

(o-, m-, p-)

Benzene

(B)

Toluene

(T)

Separation of Dioxines

Polychlorodibenzo-1,4-dioxins (pCDDs) have been in the focus of environmental separations due to their extreme toxicity.

The pCDDs are usually present as a mixture of isomers. The mixture must be separated in order to evaluate the biological

efects of each isomer. The pCDD isomers can be separated by utilizing hydrophobic, charge transfer and dipole-dipole

interactions. COSMOSIL PYE retains symmetrical isomers more strongly. In COSMOSIL NPE, on the other hand, isomers

with a strong dipole moment are retained preferentially. Both COSMOSIL PYE and NPE offer special resolutions that are

beyond the possibilities of conventional ODS columns as shown below.

Column size

Mobile phase

Flow rate

Temperature

Detection

Sample

4.6mmI.D. x 150mm

PYE: 100%-Methanol

NPE: Methanol:Water=80:20

ODS: Methanol:Water=90:10

PYE: 2.0ml/min

NPE, ODS: 1.0ml/min

30oC

UV 235nm

Dibenzo-1,4-dioxin

COSMOSIL 5NPECOSMOSIL 5PYE Conventional ODS COSMOSIL 5PYE Cnventional ODSCOSMOSIL 5NPECOSMOSIL 5PYE Conventional ODS

Polychrolodibenzo-1,4-dioxins are labeled by their substitution position in the figure.

For example, 1,2,6,7-Tetrachlorodibenzo-1,4-dioxin is labeled as "1267".

O

O

1

2

3

456

7

8

9 10

Dibenzo-1,4-dioxin

T

m-

o-, p-

B

COSMOSIL 5PYE

Page 4: COSMOSIL PYE and NPE - Hichrom · In COSMOSIL NPE, on the other hand, isomers with a strong dipole moment are retained preferentially. Both COSMOSIL PYE and NPE offer special resolutions

Separation of positional isomers like Benzylpyridine

Column size

Mobile phase

Flow rate

Temperature

Detection

Sample

4.6mmI.D. x 150mm

Methanol:20mmol/L KH2PO4=60:40

1.0ml/min

30oC

UV 254nm

1. 2-Benzylpyridine

2. 3-Benzylpyridine

3. 4-Benzylpyridine

COSMOSIL 5PYE COSMOSIL 5NPE Conventional ODS

NACALAI TESQUE, INC.Nijo Karasuma, Nakagyo-ku, Kyoto 604-0855, JAPAN

TEL: +81-75-251-1730

FAX: +81-75-251-1763

Web site: http://www.nacalai.com

Ordering information

Code No.

37903-11

38041-71

05867-91

34475-21

Product name

COSMOSIL PYE

Guard Column

Size

4.6mmI.D. x 10mm

10.0mmI.D. x 20mm

20.0mmI.D. x 20mm

20.0mmI.D. x 50mm

For research use only, not intended for diagnistic or drug use.

Product name

COSMOSIL PYE

Packed Column

Size

1.0mmI.D. x 150mm

2.0mmI.D. x 150mm

2.0mmI.D. x 250mm

4.6mmI.D. x 150mm

4.6mmI.D. x 250mm

10.0mmI.D. x 250mm

20.0mmI.D. x 250mm

Code No.

02851-71

38042-61

34450-31

37837-91

37989-11

37996-11

38044-41

Code No.

37904-01

38045-31

05868-81

05869-71

Product name

COSMOSIL NPE

Guard Column

Size

4.6mmI.D. x 10mm

10.0mmI.D. x 20mm

20.0mmI.D. x 20mm

20.0mmI.D. x 50mm

Other size may be available. Please enquire!!

Product name

COSMOSIL NPE

Packed Column

Size

1.0mmI.D. x 150mm

2.0mmI.D. x 150mm

2.0mmI.D. x 250mm

4.6mmI.D. x 150mm

4.6mmI.D. x 250mm

10.0mmI.D. x 250mm

20.0mmI.D. x 250mm

Code No.

05897-01

34328-51

34379-91

37902-21

37990-71

05469-11

38046-21

Separation of geometrical isomers like Carvylacetate

Column size

Mobile phase

Flow rate

Temperature

Detection

Sample

4.6mmI.D. x 150mm

70% methanol

1.0ml/min

30oC

UV 215nm

1. Carvylacetate (cis, trams)

COSMOSIL 5PYE COSMOSIL 5NPE

O

COCH3

N

Separation of Fluorides

Column size

Mobile phase

Flow rate

Temperature

Detection

4.6mmI.D. x 150mm

NPE: 40% methanol

ODS: 50% methanol

1.0ml/min

30oC

UV 215nm

Sample 1. Benzene

2. Fluorobenzene

3. o-Difluorobenzene

COSMOSIL 5NPE Conventional ODS

(3.0 g)

(1.0 g)

(1.0 g)

Hichrom Limited1 The Markham Centre, Station RoadTheale, Reading, Berks, RG7 4PETel: 0118 930 3660Fax: 0118 932 3484Web site: www.hichrom.co.ukEmail: [email protected]


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