+ All Categories
Home > Documents > Alcohol Biomarkers by UHPLC-MS/MS - Winlab · Ethyl glucuronide (EtG) Time (mins) %B 0.0 0 0.5 20...

Alcohol Biomarkers by UHPLC-MS/MS - Winlab · Ethyl glucuronide (EtG) Time (mins) %B 0.0 0 0.5 20...

Date post: 01-Oct-2018
Category:
Upload: buidung
View: 215 times
Download: 0 times
Share this document with a friend
12
Conditions Column: ACE Excel 1.7 C18 Dimensions: 100 x 2.1 mm Part Number: EXL-171-1002U Mobile Phase: A: 1 mM ammonium fluoride B: MeCN Flow Rate: 0.4 mL/min Injection: 1 μL Temperature: 40 °C Detection: AB SCIEX triple quad 5500 Negative ESI MRM Source temperature: 750 °C IonSpray voltage: -4500 V Alcohol Biomarkers by UHPLC-MS/MS Application #AN1910 1. Ethyl glucuronide (EtG) Time (mins) %B 0.0 0 0.5 20 1.5 20 2.0 100 4.0 100 4.5 0 Transitions Quantifiers EtS 124.8 → 79.9 EtG 221 → 85 Qualifiers EtS 124.8 → 97 EtG 221 → 75 Reproduced with permission of Biotage GB Ltd, UK 1 2 Fluoride counter-ion thought to enhance negative ESI response Detection limit ~ 1ng/ml in oral fluid 2. Ethyl sulphate (EtS) Australia & New Zealand contact: [email protected] or call +61 7 3205 1209
Transcript

Conditions

Column: ACE Excel 1.7 C18 Dimensions: 100 x 2.1 mm Part Number: EXL-171-1002U

Mobile Phase: A: 1 mM ammonium fluoride B: MeCN Flow Rate: 0.4 mL/min Injection: 1 µL Temperature: 40 °C Detection: AB SCIEX triple quad 5500 Negative ESI MRM Source temperature: 750 °C IonSpray voltage: -4500 V

Alcohol Biomarkers by UHPLC-MS/MS

Application #AN1910

1. Ethyl glucuronide (EtG)

Time (mins) %B

0.0 0 0.5 20 1.5 20 2.0 100 4.0 100 4.5 0

Transitions Quantifiers EtS 124.8 → 79.9 EtG 221 → 85 Qualifiers EtS 124.8 → 97 EtG 221 → 75

Reproduced with permission of Biotage GB Ltd, UK

1

2

Fluoride counter-ion thought to enhance negative ESI response

Detection limit ~ 1ng/ml in oral fluid

2. Ethyl sulphate (EtS)

Australia & New Zealand contact: [email protected] or call +61 7 3205 1209

Conditions

Column: ACE Excel 1.7 SuperC18 Dimensions: 50 x 3.0 mm Part Number: EXL-1711-0503U

Mobile Phase: A: 0.1% ammonia in H2O B: 0.1% ammonia in MeCN Flow Rate: 1 mL/min Injection: 0.7 µL Temperature: 20 °C Detection: UV, 230 nm

Fast Analysis of β-Blockers at High pH

Application #AN2160

Time (mins) %B

0.0 30 4.3 55 5.0 55 6.0 30

Post time 3 mins

min 1 2 3 4

mAU

0

20

40

60

80

100

120

140

160

1

4

5

6

7

2

3

1. Atenolol

3. Pindolol

7. Propranolol

4. Metoprolol

2. Acebutalol

6. Carvedilol

5. Oxprenolol

4 3 2 1 0 min

Australia & New Zealand contact: [email protected] or call +61 7 3205 1209

Conditions

Column: ACE Excel 1.7 C18-AR Dimensions: 100 x 2.1 mm Part Number: EXL-179-1002U

Mobile Phase: A: 2 mM ammonium acetate, 0.1% formic acid in H2O B: 2 mM ammonium acetate, 0.1% formic acid in MeOH Flow Rate: 0.4 mL/min Injection: 10 µL Temperature: 40 °C Detection: XEVO TQS triple quad MS Desolvation temperature: 500 °C Ion source temperature: 150 °C Positive mode ESI, MRM

Thyroid Hormones by LC-MS/MS (II)

Application #AN2180

1. T3 (Tri-iodothyronine)

3. rT3 (Reversed tri-iodothyronine)

2. T4 (Thyroxine)

Time (mins) %B

0.0 60 3.0 77 3.1 60

Reproduced with permission of Biotage GB Ltd, UK

1

3

2

TIC

Analyte Q1 (Da) Q3 (Da)

T3 651.8 605.8 (651.8) (507.8) (651.8) (478.9)

rT3 651.8 605.8 (651.8) (507.8) (651.8) (478.9)

T3/rT3-d6 I.S. 657.8 611.8 T4 777.7 731.7

(777.7) (351) (777.7) (633.8)

Australia & New Zealand contact: [email protected] or call +61 7 3205 1209

Conditions

Column: ACE Excel 1.7 C18 Dimensions: 100 x 2.1 mm Part Number: EXL-171-1002U

Mobile Phase: A: 5 mM ammonium acetate in H2O B: 5 mM ammonium acetate in MeOH Flow Rate: 0.3 mL/min Injection: 10 µL Temperature: 40 °C Detection: MS Quattro Premier XE triple quad MRM, positive and negative ESI mode Desolvation temperature: 450 °C Ion source temperature: 150 °C Collision gas pressure: 3.5 x 100-4 mbar

Drugs of Abuse Screen by

UHPLC-MS/MS

Application #AN2190

Page 1 of 2

Time (mins) %B

0.0 10 10.0 90 11.9 90 13.4 10 13.5 10

Reproduced with permission of Biotage GB Ltd, UK

Australia & New Zealand contact: [email protected] or call +61 7 3205 1209

Drugs Of Abuse Screen By

UHPLC-MS/MS

Application #AN2190

Page 2 of 2

Reproduced with permission of Biotage GB Ltd, UK

Peak Analyte Rt Q1 (Da) Q3 (Da) Peak Analyte Rt Q1 (Da) Q3 (Da)

1 Oxymorphone 2.62 302.2 198.1 27 Bromazepam 6.95 316.1 182.1 2 Morphine-d3 2.82 289.2 201.0 28 Ketamine 7.21 238.1 124.9 3 Morphine 2.95 286.2 201.0 29 Clonazepam 7.26 316.1 270.1 4 Hydromorphone 3.25 286.2 185.1 30 Nitrazepam 7.26 282.2 236.1 5 Amphetamine-d5 3.62 141.0 123.9 31 Alpha-hydroxytriazolam 7.34 359.1 331.1 6 Amphetamine 3.65 136.0 118.9 32 Flunitrazepam 7.34 314.2 268.2 7 Dihydrocodeine 3.66 302.2 199.1 33 Alpha-hydroxyalprazolam 7.54 325.2 297.1 8 MDA 3.67 180.1 105.0 34 Estazolam 7.56 295.2 267.2 9 MDMA 3.75 194.1 163.0 35 Zolpidem 7.73 308.2 235.1

10 Methamphetamine 3.8 150.0 90.9 36 Triazolam 7.77 343.0 308.1 11 Oxycodone 4.03 316.2 241.2 37 2-Hydroxyethylflurazepam 7.77 333.2 109.0 12 MDEA 4.12 208.2 163.0 38 Lorazepam 7.80 321.1 275.1 13 BZE-d3 4.15 293.1 171.0 39 Oxazepam 7.82 287.2 241.0 14 BZE 4.17 290.1 168.0 40 Alprazolam 7.85 309.2 281.2 15 6-MAM 4.48 328.2 165.1 41 Methadone 7.99 310.2 265.2 16 Codeine 4.59 300.3 215.1 42 Temazepam 8.05 301.1 255.1 17 Norfentanyl 4.71 233.1 84.0 43 Nordiazepam 8.44 271.1 139.9 18 7-Amino-clonazepam 4.77 286.2 121.0 44 Midazolam 8.61 326.2 291.2 19 Hydrocodone 4.94 300.2 199.1 45 Diazepam-d5 8.63 290.2 154.0 20 7-Amino-flunitrazepam 5.34 284.2 135.0 46 Diazepam 8.67 285.2 154.0 21 Cocaine 5.99 304.2 182.0 47 Flurazepam 8.68 388.2 315.1 22 Norbuprenorphine 6.47 414.3 101.0 48 Fentanyl 8.85 337.3 105.0 23 PCP 6.49 244.2 159.9 49 THC-COOH-d3 9.98 348.2 302.2 24 Zaleplon 6.55 306.2 264.2 50 THC-COOH 10.01 345.2 299.2 25 EDDP 6.58 278.2 234.2 51 Buprenorphine 11.70 468.3 101.0 26 Norketamine 6.9 224.1 124.9

Australia & New Zealand contact: [email protected] or call +61 7 3205 1209

Conditions

Column: ACE 3 C18-Amide ACE Excel 1.7 C18-Amide Dimensions: 250 x 2.1 mm 50 x 3.0 mm Part Number: 250 x 2.1 mm (EXL-1112-2502U), 50 x 3 mm (EXL-1712-0503U) Mobile Phase: 20 mM H3PO4 in MeOH/H2O (40:60 v/v) Flow Rate: 0.21 mL/min (250 x 2.1 mm) 0.8 mL/min (50 x 3.0 mm) Injection: 5 µL (250 x 2.1 mm) 2 µL (50 x 3.0 mm) Temperature: 20 °C Detection: UV, 210 nm

Fast Separation of Organic Acids

Application #AN2200

min 5 10 15 20 25 30 35 40

mAU

0

25

50

75

100

125

150

175

200

1

2

3

4

5

mAU

0

25

50

75

100

125

150

175

1

2

3

4

5

min 5 10 15 20 25 30 35 40

4. Cinnamic acid

1. Sinapic acid

3. 3,4-Dimethoxycinnamic acid

2. Ferulic acid

5. 4-Methoxycinnamic acid

ACE 3 C18-Amide

ACE Excel 1.7 C18-Amide

0 I

0 I

Australia & New Zealand contact: [email protected] or call +61 7 3205 1209

Conditions

Column: ACE Excel 1.7 C18 Dimensions: 50 x 3.0 mm Part Number: EXL-171-0503U

Mobile Phase: A: 10 mM ammonium acetate pH 6.0 in H2O B: 10 mM ammonium acetate pH 6.0 in MeOH/H2O (90:10 v/v) Flow Rate: 0.51 mL/min Injection: 0.7 µL (50 x 3.0 mm) Temperature: 40 °C Detection: UV, 230 nm

Fast Analysis of Paracetamol and

Related Substances (I)

Application #AN2210

1. 4-Aminophenol 2. Hydroquinone 3. Paracetamol 4. 2-Acetamidophenol 5. Phenol 6. 4-Nitrophenol 7. 2-Nitrophenol 8. 4-Chloroacetanilide

Time (mins) %B

0.00 5 0.08 5 5.08 95 6.76 95 7.09 5 10.00 5

For enhanced resolution of paracetamol and related compounds, see AN2220.

0 2 4 6

mAU

0

20

40

60

80

100

1

2

3

4

5

7 6

8

2 4 6 min 0

Australia & New Zealand contact: [email protected] or call +61 7 3205 1209

Conditions

Column: ACE Excel 1.7 C18 Dimensions: 100 x 3.0 mm Part Number: EXL-171-1003U Mobile Phase: A: 10 mM ammonium acetate pH 6.0 in H2O B: 10 mM ammonium acetate pH 6.0 in MeOH/H2O (90:10 v/v) Flow Rate: 0.51 mL/min Injection: 1.4 µL Temperature: 40 °C Detection: UV, 230 nm

Enhanced Resolution of Paracetamol

and Related Substances

Application #AN2220

Time (mins) %B

0.00 5 0.21 5 10.23 95 13.56 95 14.16 5 20.24 5

1. 4-Aminophenol 2. Hydroquinone 3. Paracetamol 4. 2-Acetamidophenol 5. Phenol 6. 4-Nitrophenol 7. 2-Nitrophenol 8. 4-Chloroacetanilide

For enhanced speed of paracetamol and related compounds, see AN2210.

0 2.5 5 7.5 10 12.5

mAU

0

20

40

60

80

100

1

2

3

4

5

7 6

8

2.5 5 7.5 10 12.5 min 0

Australia & New Zealand contact: [email protected] or call +61 7 3205 1209

Conditions

Column: ACE Excel 1.7 C18-Amide Dimensions: 50 x 3.0 mm Part Number: EXL-1712-0503U

Mobile Phase: A: 0.1% formic acid in H2O B: 0.1% formic acid in MeCN Flow Rate: 1.3 mL/min Injection: 1 µL Temperature: 45 °C Detection: UV, 260 nm

Fast Separation of Vanillin Compounds

Application #AN2240

4. 4-Hydroxybenzaldehyde

1. Vanillic acid

3. Vanillin

2. 4-Hydroxybenzoic acid

Time (mins) %B

0.00 25 1.32 75 1.49 75 1.60 25

min 0.2 0.4 0.6 0.8 1 1.2 1.4

mAU

0

50

100

150

200

250

1

2

3

4

5

6

7

8

7. Ethyl vanillin

6. o-Vanillin

5. Guaicol

8. Eugenol

0

Australia & New Zealand contact: [email protected] or call +61 7 3205 1209

Conditions

Column: ACE Excel 1.7 C18 Dimensions: 100 x 2.1 mm Part Number: EXL-171-1002U

Mobile Phase: A: 2 mM ammonium acetate, 0.1% formic acid/MeCN (90:10 v/v) B: 2 mM ammonium acetate, 0.1% formic acid in MeCN (10:90 v/v) Flow Rate: 0.5 mL/min Injection: 10 µL Temperature: 40 °C Detection: AB SCIEX triple quad 5500 Negative ESI MRM Source temperature: 450 °C IonSpray voltage: -2400 V

Perfluorinated Compounds in Water by

LC-MS/MS

Application #AN2260

Reproduced with permission of Biotage GB Ltd, UK. For extraction conditions see Biotage Application Note AN839

XIC of -MRM (9 pairs): Exp 1, 212.900/168.900 amu Expected RT: 1.0 ID: HFBA 1 from Sample 5 (PFA8 5ng/mL) of 150224_standards.wiff (... Max. 3.8e4 cps.

0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5Time, min

0.0

5.0e4

1.0e5

1.5e5

2.0e5

2.5e5

3.0e5

3.5e5

4.0e5

4.5e5

5.0e5

5.5e5

6.0e5

6.5e5

7.0e5

7.5e5

8.0e5

8.5e5

Inte

nsity

, cps

0.86

0.99 1.20 1.250.76

1

2

3

4

5

6

7

Transitions 1. Perfluorohexanoic acid (m/z 313.0 → 268.9) 2. Perfluorobutanesulfonic acid (m/z 299.0 → 79.9) 3. Perfluorooctanoic acid (m/z 413.0 → 368.9) 4. Perfluorohexanesulfonic acid (m/z 399.0 → 80.0) 5. Perfluorononanoic acid (m/z 463.0 → 419.0) 6. Perfluorodecanoic acid (m/z 513.0 → 469.0) 7. Perfluorooctanesulfonic acid (m/z 499.0 → 80.0)

Time (mins) %B

0.0 25 0.5 25 3.5 70 4.0 100 5.5 100 6.0 25 9.0 25

4.0 3.0 2.5 2.0 3.5 0.5 0 1.5 1.0 4.5 Time, mins

Australia & New Zealand contact: [email protected] or call +61 7 3205 1209

Conditions

Column: ACE Excel 1.7 C18-PFP Dimensions: 2 x 100 x 3.0 mm (coupled) Part Number: 2 x EXL-1710-1003U

Mobile Phase: A: 0.1% formic acid in H2O B: 0.1% formic acid in MeCN Flow Rate: 0.8 mL/min Injection: 2 µL Temperature: 80 °C Detection: UV, 254 nm

Ultra Resolution Separation of the

Natural Product Ginkgo Biloba

Application #AN2270

1. Ginkgo Biloba

Time (mins) %B

0.0 5 0.72 5 15.72 50 18.72 100 20.72 100 22.72 5

min 2 4 6 8 10 12

mAU

-5

0

5

10

15

20

25

30

Australia & New Zealand contact: [email protected] or call +61 7 3205 1209

Conditions

Column: ACE Excel 1.7 CN-ES Dimensions: 50 x 3.0 mm Part Number: EXL-1713-0503U

Mobile Phase: A: 0.1% formic acid in H2O B: 0.1% formic acid in MeCN Flow Rate: 0.7 mL/min Injection: 0.5 µL Temperature: 30 °C Detection: UV, 240 nm

Separation of Aspirin and Related

Substances

Application #AN2280

1. 2-Acetamidophenol 2. 4-Hydroxyisophthalic acid 3. Acetanilide 4. Salicylamide 5. Aspirin 6. Phenacetin 7. Salicylic acid 8. Acetylsalicylsalicylic acid 9. Salsalate

Time (mins) %B

0 5 5 90 6 90

6.5 5

min 1 2 3 4

4

5

6

7

8

9

2

3

1

2 1 4 min 3

Gordon
Text Box
In Australia and New Zealand WINLAB PTY LTD PO Box 5007, Brendale, QLD 4500, Australia Ph: +61 7 3205 1209 Email: [email protected] Web: www.winlab.com.au

Recommended