Rtx11 12 - 708 751

HPLC CHROMATOGRAMS
HPLC Chromatograms by Column Phase Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .709 Environmental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .710-718

Aldehydes, Explosives, Herbicides, Ketones, Pesticides, Polycyclic Aromatic Hydrocarbons
Foods & Flavors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .719-735

Dietary Supplements, Drug Residues, Flavor Compounds, Food Contaminants, Preservatives, Sugars, Vitamins
Pharmaceutical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .736-743
Admixed Drugs, Analgesics, Antiarrhythmics, Antiasthmatics, Antibiotics, Anti-Diabetic, Corticosteroids, Famotidine, Lactulose Concentrate, Potential Genotoxic Impurities, Steroids, Xanthines
Biochemical/Clinical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .744-746
Amino Acids, Catecholamines, Nucleic Acid Bases, Nucleosides, Nucleotides, Oxytocin, Peptides, Proteins, Purines/Pyrimidines
Clinical/Forensic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .747-751
Alcohol Metabolites, Amphetamines, Benzodiazepines, Cocaine, Diuretics, Opiates, Pain Management Drugs, THC
Website : www.chromtech.net.au E-mail : info@chromtech.net.au TelNo : 03 9762 2034 . . . in AUSTRALIA
Mar 2011
HPLC CHROMATOGRAMS
HPLC Chromatograms by Column Phase

HPLC Chromatograms by Column Phase (Alphabetical Order)
Allure AK
carbonyls . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .181, 710
Ultra C8
explosives . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .711 oxycodone . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .738 vanillin & ethyl vanillin . . . . . . . . . . . . . . . . . . . . . . .728 vitamins . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .733
Allure Basix
herbicides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .714
Allure Biphenyl
antibiotics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .740 corticosteroids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .741 steroids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .742
Ultra Carbamate
food contaminants (carbamates) . . . . . . . . . . . . . . .719
Ultra Cyano
antiarrhythmics . . . . . . . . . . . . . . . . . . . . . . . . . . . . .739
Allure C18
herbicides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .712 pesticides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .716
Ultra IBD
antiarrhythmics . . . . . . . . . . . . . . . . . . . . . . . . . . . . .739 antibiotics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .740, 741 diflubenzuron (pesticide) . . . . . . . . . . . . . . . . . . . . .716 glyburide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .741 nucleosides, nucleotides, & nucleic acid bases . . . .744 vitamins . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .732
Allure Organic Acids

fruit juice acids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .531
Allure PFP Propyl

antibiotics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .723 benzodiazepines . . . . . . . . . . . . . . . . . . . . . . . . . . . . .751 catecholamines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .745 cocaine, ecgonine methyl ester . . . . . . . . . . . . . . . . .750 nucleic acid bases . . . . . . . . . . . . . . . . . . . . . . . . . . . .744 opiates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .748
Ultra PFP
purines, pyrimidines . . . . . . . . . . . . . . . . . . . . . . . . .745
Ultra Phenyl
guaifenesin, codeine . . . . . . . . . . . . . . . . . . . . . . . . . .743
Pinnacle DB Aqueous C18

food contaminants . . . . . . . . . . . . . . . . . . . . . . .720, 722 pesticides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .720, 722
Ultra Quat
paraquat, diquat . . . . . . . . . . . . . . . . . . . . . . . . .189, 715
GC & HPLC Chromatograms
Ultra II Aqueous C18

dietary supplements . . . . . . . . . . . . . . . . . . . . . . . . . .729 herbicides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .713 melatonin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .729 organic acids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .729 vitamins . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .734
Compound Index
starting on page 752
Pinnacle DB Biphenyl
drug residues . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .725 steroids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .742
Pinnacle DB C18
vanilla bean extracts . . . . . . . . . . . . . . . . . . . . . . . . . .727 xanthines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .743
Ultra II Aromax
explosives . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .485, 711 famotidine and USP impurities . . . . . . . . . . . . . . . .736 potential genotoxic impurities . . . . . . . . . . . . . . . . .737 vitamins . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .735
Pinnacle DB PAH
PAHs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .718
Pinnacle II Amino
lactulose concentrate . . . . . . . . . . . . . . . . . . . . . . . . .743 sugars . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .727
Ultra II Biphenyl
alcohol metabolites . . . . . . . . . . . . . . . . . . . . . . . . . .749 amphetamines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .750 antibiotics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .725 diuretics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .749 drug residues . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .725 drugs of abuse . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .748 NSAIDs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .723 pain managment drugs in urine . . . . . . . . . . . . . . . .747 sulfa drugs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .725 THC & metabolites . . . . . . . . . . . . . . . . . . . . . . . . . .748
Pinnacle II C18
allicin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .730 capsaicinoids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .728 morphine sulfate . . . . . . . . . . . . . . . . . . . . . . . . . . . .738 phenolic antioxidants . . . . . . . . . . . . . . . . . . . .727, 730
Pinnacle II Cyano
piperine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .728
Pinnacle II PAH
PAHs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .717
Pinnacle II Silica
hydrocodone bitartrate . . . . . . . . . . . . . . . . . . . . . . .738 tocopherols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .730
Ultra II C18
vitamins . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .733
Ultra Aqueous C18

amino acids (aromatics) . . . . . . . . . . . . . . . . . . . . . .745 analgesics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .737 carboxylic acids . . . . . . . . . . . . . . . . . . . . . . . . . . . . .726 food contaminants . . . . . . . . . . . . . . . . . . . . . . .721, 722 herbicides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .714 pesticides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .721 phenethyl glucosinolate . . . . . . . . . . . . . . . . . . . . . . .730 sudan dyes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .722 vitamins . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .731
Ultra II Carbamate
food contaminants . . . . . . . . . . . . . . . . . . . . . . . . . . .719 pesticides (carbamates) . . . . . . . . . . . . . . . . . . . . . . .719
Viva C18
oxytocin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .746 peptides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .745 proteins . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .746
Chromatogram Search Tool

Search by compound name, synonym, CAS # or keyword
Ultra C18
acetaminophen, narcotic analgesics . . . . . . . . . . . . .738 aldehydes, ketones . . . . . . . . . . . . . . . . . . . . . . . . . . .710 beclomethasone . . . . . . . . . . . . . . . . . . . . . . . . . . . . .739 corticosteroids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .741 drug residues . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .724 herbicides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .712 hydrocodone bitartrate, acetaminophen . . . . . . . . .743 nitrofuran metabolites . . . . . . . . . . . . . . . . . . . . . . . .724 vitamins (fat soluble) . . . . . . . . . . . . . . . . . . . . . . . . .732
www.restek.com/chromatograms
800-356-1688 or 814-353-1300
www.restek.com
709
Mar 2011
HPLC CHROMATOGRAMS | ENVIRONMENTAL
Aldehydes, Ketones
Carbonyls by CARB Method 1004 on Allure AK
Sample: Inj.: Conc.:
10L 3g/mL each analyte, as aldehyde/ketone Sample diluent: acetonitrile Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Allure AK 9159525-700 200mm x 4.6mm 5m 60 A) water : B) acetonitrile Time (min.) %B 0 60 8 70 10 100 1.5mL/min. 30C UV @ 360nm
Peak DNPH derivatives of: 1. formaldehyde 2. acetaldehyde 3. acrolein 4. acetone 5. propionaldehyde 6. crotonaldehyde 7. methacrolein 8. butyraldehyde 9. methylethylketone 10. benzaldehyde 11. valeraldehyde 12. m-tolualdehyde 13. hexaldehyde
Ret. Time (min.) 4.74 5.78 6.86 7.09 7.31 8.19 8.55 8.79 9.06 10.03 10.39 11.08 11.36
Flow: Temp.: Det.:
LC_EV0393
Aldehydes and Ketones (DNPH derivatives) on Ultra C18 (40C)

1
Sample: Inj.: Conc.: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase:
10L 3.0g/mL each derivative Ultra C18 9174565 150mm x 4.6mm 5m 100
Peak List: DNPH derivatives of: 1. formaldehyde 2. acetaldehyde 3. acetone 4. acrolein 5. propionaldehyde 6. crotonaldehyde 7. MEK 8. methacrolein 9. butyraldehyde 10. benzaldehyde 11. valeraldehyde 12. m-tolualdehyde 13. hexanaldehyde
4 3 5 6 7 8 9
Flow rate: Det.: Temp.:
Solvent A: water Solvent B: acetonitrile Solvent C: tetrahydrofuran 50-30% A/30-65% B/20-5% C, 0-15 min. 1.5mL/min. UV @ 365nm 40C
10
11 12 13
6 LC_0036
10
12
14 min.
710 www.restek.com
Website : www.chromtech.net.au E-mail : info@chromtech.net.au TelNo : 03 9762 2034 . . . in AUSTRALIA Mar 2011
Explosives
Explosives EPA Method 8330B Ultra II Aromax
1. 2. 3. 4. 5. 6. 7. 8. 9. HMX RDX nitroglycerin nitrobenzene 4-amino-2,6-dinitrotoluene 3,5-dinitroaniline 2-nitrotoluene 2-amino-4,6-dinitrotoluene 3-nitrotoluene 10. 11. 12. 13. 14. 15. 16. 17. PETN 4-nitrotoluene 1,3-dinitrobenzene 2,6-dinitrotoluene tetryl 2,4-dinitrotoluene 1,3,5-trinitrobenzene 2,4,6-trinitrotoluene
NEW!
Nitroaromatics and Nitramine Explosives by HPLC, EPA 8330B (cat.# 33204) Inj.: 10L Conc.: 10g/mL each component Sample diluent: methanol Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Flow: Temp.: Det.: Ultra II Aromax 9607575 250mm x 4.6mm 5m 100 Shimadzu Prominence UFLCXR water:methanol, 35:65 (v/v) 1.2mL/min. 30C UV @ 254nm and 210nm
Sample:
LC_EV0484
Explosives EPA Method 8330B Ultra C8
1. 2. 3. 4. 5. 6. 7. 8. 9.
HMX RDX nitroglycerin nitrobenzene 4-amino-2,6-dinitrotoluene 3,5-dinitroaniline 2-nitrotoluene 2-amino-4,6-dinitrotoluene 3-nitrotoluene
10. 11. 12. 13. 14. 15. 16. 17.
PETN 4-nitrotoluene 1,3-dinitrobenzene 2,6-dinitrotoluene tetryl 2,4-dinitrotoluene 1,3,5-trinitrobenzene 2,4,6-trinitrotoluene
NEW!
Sample:
Nitroaromatics and Nitramine Explosives by HPLC, EPA 8330B (cat.# 33204) Inj.: 10L Conc.: 50g/mL each component Sample diluent: methanol Column: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Flow: Temp.: Det.: Ultra C8 cat.# 9103575 250mm x 4.6mm 5m 100 Shimadzu Prominence water:methanol, 52:48 (v/v) 1.2mL/min. 30C UV @ 254nm and 210nm
LC_EV0485
www.restek.com
711
Mar 2011
Herbicides
Herbicides (Phenylurea) on Ultra C18
Peak List: 1. tebuthiuron 2. thidiazuron 3. monuron 4. fluometuron 5. diuron 6. propanil 7. siduron 8. linuron 9. carbazole 10. diflubenzuron Conc. (g/mL or ppm) 2 2 5 2 2 2 2 2 5 2 Sample: Inj.: Conc.: Sample diluent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase:
20L see peak list acetonitrile Ultra C18 9174565 150mm x 4.6mm 5m 100 A: 25mM phosphate buffer, pH 2.5 B: acetonitrile Time (min.) %B 0 40 8 40 14 55 18 55 19 40 1.5mL/min. ambient UV @ 245nm
Flow: Temp.: Det.:
LC_0319
Herbicides on Allure C18
Peak List: 1. cyanazine 2. methabenzthiazuron 3. chlortoluron 4. secbumeton 5. isoproturon 6. diuron 7. linuron 8. flusilazole 9. ethofumesate 10. neburon 11. pendimethalin
Ret. Time (min.) 12.04 13.88 14.59 15.74 16.18 16.78 22.48 24.29 24.53 25.74 31.46
Sample: Inj.: Conc.: Diluent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase:
5L custom mix approx. 20g/mL each acetonitrile Allure C18 9164565 150mm x 4.6mm 5m 60 A: water B: acetonitrile Time (min.) %B 0 20 10 40 15 40 26 80 34 80 34.1 20 1.2mL/min. ambient UV @ 220nm
Flow: Temp.: Det.:
LC_0309
712 www.restek.com
Herbicides
Phenoxyacid Herbicides on Ultra II Aqueous C18 (LC/MS/MS)
NEW!
Peaks RT (min.) 1. Dicamba 1.14 2. Bentazon 1.32 3. 2,4-D 3.10 4. 3,5-DCBA 3.10 5. 4-Nitrophenol 3.10 6. MCPA 3.16 7. Dichlorprop 4.02 8. 2,4,5-T 4.46 9. Dinoseb 5.03 10. 2,4-DB 5.18 11. 2,4,5-TP 5.20 12. Acifluorfen 5.67 13. Pentachlorophenol 6.20 MRM 1 219.0 175.0 239.0 132.0 218.9 161.0 189.0 144.8 138.1 108.1 199.0 141.0 233.0 161.0 252.9 194.9 239.0 133.9 247.0 161.0 266.9 195.0 359.9 316.1 264.8 35.0 MRM 2 221.0 177.0 239.0 175.0 220.9 163.0 189.0 59.0 138.1 46.0 201.0 143.0 235.0 163.0 254.9 196.9 239.0 193.8 249.0 163.0 266.9 159.0 359.9 195.0 264.8 37.0
Column Dimensions: Particle Size: Pore Size: Temp.: Sample Diluent: Conc.: Inj. Vol.: Mobile Phase A: B:
Ultra II Aqueous C18 (cat.# 9608312) 100 mm x 2.1 mm ID 3 m 100 35 C phenoxyacid herbicides acetonitrile 100 ppb 10 L 10mM ammonium acetate in water 10mM ammonium acetate in methanol Time (min.) 0 8 12 14.8 15 %A 80 10 0 0 80 %B 20 90 100 100 20
LC_EV0511
Flow: 0.5 mL/min. Detector Applied Biosystems/MDS Sciex LC/MS/MS Model #: 4000 QTRAP LC/MS/MS System Ion Source: Electrospray Ion Mode: ESIIon Spray Voltage: -4.2 kV ESI Voltage: -4.2 V Gas 1: 50 psi (344.7 kPa) Gas 2: 60 psi (413.7 kPa) Source Temp.: 600 C Mode: MRM Instrument Applied Biosystems/MDS Sciex LC/MS/MS System Acknowledgement Work performed at Applied Biosystems
Get More!
Environmental Solutions Online
www.restek.com/enviro
www.restek.com
713
Mar 2011
Herbicides
Phenoxyacid Herbicides on Ultra Aqueous C18
Mix A and Mix B 1. picloram 2. chloramben 3. 4-nitrophenol 4. dicamba 5. bentazon 2,4-dichlorophenyl acetic acid (SS) (not included) 7. 2,4-D 8. MCPA 9. 3,5-dichlorobenzoic acid 10. MCPP 11. dichlorprop 12. 2,4,5-T 13. 2,4-DB 14. 2,4,5-TP (Silvex) 15. acifluorfen 1,4-dichlorobenzene (IS) (not included) 17. dinoseb 18. pentachlorophenol
Sample: Sample:
Chlorinated Acids by HPLC, Mix A (cat.# 32431), or Chlorinated Acids by HPLC, Mix B (cat.# 32430) 1,000g/mL each component in acetonitrile Inj.: 10L Conc.: 10ppm each analyte Sample diluent: acetonitrile Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Ultra Aqueous C18 9178565 150mm x 4.6mm 5m 100 A) 0.05% H3PO4 B) acetonitrile Time (min.) %B 0 20.0 28 80.0 33 90.0 34 20.0 1.0mL/min. ambient UV @ 225nm
Flow: Temp.: Det.:
LC_EV0356
LC_EV0355
Phenoxyacid Herbicides on Allure Basix

Mix A and Mix B 1. picloram 2. chloramben 3. 4-nitrophenol 4. dicamba 5. bentazon 2,4-dichlorophenyl acetic acid (SS) (not included) 7. 2,4-D 8. MCPA 9. 3,5-dichlorobenzoic acid 10. MCPP 11. dichlorprop 12. 2,4,5-T 13. 2,4-DB 14. 2,4,5-TP (Silvex) 15. acifluorfen 1,4-dichlorobenzene (IS) (not included) 17. dinoseb 18. pentachlorophenol Sample: Sample:
Chlorinated Acids by HPLC, Mix A (cat.# 32431), or Chlorinated Acids by HPLC, Mix B (cat.# 32430) 1,000g/mL each component in acetonitrile Inj.: 10L 10ppm each analyte Conc.: Sample diluent: acetonitrile Allure Basix 9161565 150mm x 4.6mm 5m 60 A) 0.05% H3PO4 B) acetonitrile Time (min.) %B 0 20.0 28 80.0 33 90.0 34 20.0 1.0mL/min. ambient UV @ 225nm
Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase:
Flow: Temp.: Det.:
LC_EV0357 LC_EV0358
714 www.restek.com
Herbicides
Paraquat and Diquat on Ultra Quat
1 2
Peak List: 1. diquat 2. paraquat
Peak time (min.) 7.5 8.8
min.
diquat 308nm
100g/mL
Sample: Inj.: Conc.:
20L 20ppm each component (above); 20g/mL, 40g/mL, and 100g/mL each component at 308nm (left) and at 257nm (right) Sample diluent: water Column: Cat.#: Dimensions: Particle size: Conditions: Mobile phase: Flow: Temp.: Det.: Ultra Quat 9181565 150mm x 4.6mm 5m Ultra Quat Reagent Solution (cat.# 32441): acetonitrile, 95:5 (v/v) 1.0 mL/min. 27C UV @ 257nm (paraquat) UV @ 308nm (diquat)
paraquat 257nm
100g/mL
40g/mL
40g/mL
20g/mL
20g/mL LC_0321
min.
Paraquat and Diquat on Ultra Quat

Sample: Inj.: Conc.: Sample diluent: Sample temp.: Column: Cat.#: Dimensions: Particle size: Pore size:
Fast, sensitive LC/MS/MS analysis!
Peak List 1. diquat 2. paraquat
10L 5g/mL each component DI water ambient Ultra Quat 5181352 50mm x 2.1mm 3m 100 10mM heptafluorobutyric acid:acetonitrile, 95:5 (v/v) 0.3mL/min. ambient Applied Biosystems/MDS SCIEX API 3200 MS/MS system electrospray positive 600C 5,500V 3V 15psi (103kPa) 70psi (483kPa) 60psi (414kPa) (MRM) unit resolution 200 ms DP (V) 30 20 Collision Energy (eV) 30 20
paraquat dichloride [CAS# 1910-42-5]
Conditions: Mobile phase: Flow: Temp.: Det.: Interface: Ion Mode: Temp.: Ion Spray voltage: Collision exit potential: Curtain Gas: Gas supply 1: Gas supply 2: Quantitation: Q1/Q3: Dwell time:
diquat dibromide [CAS # 85-00-7]
LC_EV0383
*Data courtesy of Houssain El Aribi, Ph.D., LC/MS Product and Application Specialist, MDS SCIEX, 71 Four Valley Drive, Concord, Ontario, Canada, L4K 4V8
Precursor Ion Fragment Ion (amu) (amu) diquat, 183+ 157+ paraquat, 93 (2+) 171+
www.restek.com
715
Mar 2011
Pesticides
Pesticides on Allure C18
Peak List: 1. desisopropyl atrazine 2. desethyl atrazine 3. simazine 4. terbuthylazine desethyl 5. cyanazine 6. methabenzthiazuron 7. chlortoluron 8. atrazine 9. secbumeton 10. isoproturon 11. diuron 12. terbumeton 13. terbuthylazine 14. linuron 15. flusilazole 16. ethofumesate 17. neburon Sample: Inj.: Conc.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase
5L approx. 10ppm each pesticide acetonitrile Allure C18 9164565 150mm x 4.6mm 5m 60 A: 20mM K2HPO4, pH 7.0 B: acetonitrile Time (min.) %B 0 20 10 40 15 40 30 70 30.1 20 1.2mL/min. ambient UV @ 220nm
Flow: Temp.: Det.:
LC_0310
Diflubenzuron (Pesticide) on Ultra IBD

1
Peak List: 1. diflubenzuron 2. N,N'-bis-(chlorobenzyl)urea Sample: Inj.: Conc.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Solvent A: Flow rate: Temp.: Det.: 10L 1mg/mL water:acetonitrile (1:1, v/v) Ultra IBD 9175365 150mm x 4.6mm 3m 100
Jamie Hubler, Customer Service

water:acetonitrile (45:55, v/v) 65% 0.1M ammonium acetate pH 6.0 1.0mL/min. ambient UV @ 260nm
Restek Customer Service

2
In the U.S.
Call: 800-356-1688 (ext. 3) or 814-353-1300 (ext. 3) MondayFriday 8:00 a.m.6:00 p.m. ET Fax: 814-353-130924-hours a day Online: www.restek.com24-hours a day
Outside the U.S.

Contact your Restek representative: Refer to our list on pages 4-5 or visit our website at www.restek.com
8
LC_0081
10
12
14 min.
716 www.restek.com
Polycyclic Aromatic Hydrocarbons

Polycyclic Aromatic Hydrocarbons Pinnacle II PAH
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. naphthalene acenaphthylene acenaphthene fluorene phenanthrene anthracene fluoranthene pyrene benzo(a)anthracene chrysene benzo(b)fluoranthene benzo(k)fluoranthene benzo(a)pyrene benzo(ghi)perylene dibenzo(a,h)anthracene indeno(1,2,3-cd)pyrene * contaminant Sample: Inj.: 10L Conc.: 10g/mL each component Sample diluent: methanol Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Pinnacle II PAH 9219463 150mm x 3.2mm 4m 110 Shimadzu Prominence A: water B: methanol Time (min.) %B 0.0 75 10.0 90 22.0 100 1.0mL/min. 30C UV @ 254nm
NEW!
Baseline resolution of PAHs in methanol!
Flow: Temp.: Det.:
10
9 11 13 7 12 8 14 15 16
1 2 * 3
10
12
LC_EV0480
14
16
18
20
22
24
Polycyclic Aromatic Hydrocarbons on Pinnacle II PAH EPA 8310 18 component standard + benzo(j)fluoranthene
Peak List: Retention Time 1. naphthalene 6.19 2. acenaphthylene 7.16 3. 1-methylnaphthalene 7.78 4. 2-methylnaphthalene 8.17 5. acenaphthene 8.46 6. fluorene 8.82 7. phenanthrene 9.64 8. anthracene 10.39 9. fluoranthene 11.22 10. pyrene 11.75 11. benzo(a)anthracene 13.55 12. chrysene 13.91 13. benzo(j)fluoranthene 14.92 14. benzo(b)fluoranthene 15.27 15. benzo(k)fluoranthene 15.82 16. benzo(a)pyrene 16.35 17. dibenzo(a,h)anthracene 17.10 18. benzo(ghi)perylene 17.67 19. indeno(1,2,3-cd)pyrene 17.99 Sample: Inj.: 10L Conc.: 20g/mL each component Sample diluent: acetonitrile Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Pinnacle II PAH 9219463 150mm x 3.2mm 4m 110 Shimadzu Prominence HPLC A: purified water B: acetonitrile Time (min.) %B 0 40 7 60 16 100 18.9 100 19 40 1.2mL/min. 30C UV @ 254nm
Flow: Temp.: Det.:
LC_EV0449
www.restek.com
717
Mar 2011
Polycyclic Aromatic Hydrocarbons

EPA Method 610 Polycyclic Aromatic Hydrocarbons on Pinnacle DB PAH
Peak List: 1. naphthalene 2. acenaphthylene 3. 1-methylnaphthalene 4. 2-methylnaphthalene 5. acenaphthene 6. fluorene 7. phenanthrene 8. anthracene 9. fluoranthene 10. pyrene 11. benzo(a)anthracene 12. chrysene 13. benzo(b)fluoranthene 14. benzo(k)fluoranthene 15. benzo(a)pyrene 16. dibenzo(a,h)anthracene 17. benzo(ghi)perylene 18. indeno(1,2,3-cd)pyrene
LC_EV0469
Sample: Inj.: 2L Conc.: 20g/mL each component Sample diluent: acetonitrile Column: Cat.#: Dimensions: Particle size: Pore size: Pinnacle DB PAH 9470252 50mm x 2.1mm 1.9m 140
Conditions: Mobile phase:
A: water B: acetonitrile Time (min.) %B 0 50 1 60 3 100 5 100 0.6mL/min. 30C UV @ 254nm
Flow: Temp.: Det.:
EU 256/2005 Polycyclic Aromatic Hydrocarbons on Pinnacle DB PAH
Peak List: 1. cyclopenta(c,d)pyrene 2. benzo(a)anthracene 3. chrysene 4. 5-methylchrysene 5. benzo(j)fluoranthene 6. benzo(b)fluoranthene 7. benzo(k)fluoranthene 8. benzo(a)pyrene 9. dibenzo(a,l)pyrene 10. dibenzo(a,h)anthracene 11. benzo(ghi)perylene 12. indeno(1,2,3-cd)pyrene 13. dibenzo(a,e)pyrene 14. dibenzo(a,i)pyrene 15. dibenzo(a,h)pyrene
min.
LC_EV0470
Sample: Inj.: 2L Conc.: 20g/mL each component Sample diluent: acetonitrile Column: Cat.#: Dimensions: Particle size: Pore size: Pinnacle DB PAH 9470252 50mm x 2.1mm 1.9m 140
A: water B: acetonitrile Time (min.) %B 0 50 1 90 2 95 5 100 7 100 0.6mL/min. 30C UV @ 254nm
Flow: Temp.: Det.:
718 www.restek.com
HPLC CHROMATOGRAMS | FOODS & FLAVORS
Food Contaminants
Carbamate Pesticides on Ultra II Carbamate (LC/MS/MS)
NEW!
Peaks RT (min.) 1. Aldicarb sulfone 1.9 2. Aldicarb sulfoxide 2.2 3. Oxamyl 2.4 4. Methomyl 2.6 5. 3-Hydroxycarbofuran 3.5 6. Aldicarb 4.5 7. Propoxur 5.1 8. Carbofuran 5.3 9. Carbaryl 5.8 10. Methiocarb 7.0 Transition 1 223.1 86.1 207.1 132.1 237.1 72.1 163.1 88.1 238.1 163.1 208.1 116.0 210.1 111.0 222.1 165.2 202.1 145.1 226.1 169.2 Transition 2 223.1 148.0 207.1 89.1 237.1 90.1 163.1 106.0 238.1 181.2 208.1 88.9 210.1 168.1 222.1 123.0 202.1 127.1 226.1 121.0 Column Dimensions: Particle Size: Pore Size: Temp.: Sample Diluent: Conc.: Inj. Vol.: Mobile Phase A: B: Ultra II Carbamate (cat.# 9611312) 100 mm x 2.1 mm ID 3 m 100 35 C 531.1 Carbamate Pesticide Calibration Mixture (cat.# 32273) acetonitrile 100 ppb each pesticide 5 L 10 mM NH4OAc in water 10 mM NH4OAc in methanol Time (min.) %B 0 10 1 10 8 90 10 90 11 10 0.5 mL/min. Applied Biosystems/MDS Sciex LC/MS/MS System Applied Biosystems/MDS Sciex LC/MS/MS 4000 QTRAP LC/MS/MS system TurboIonSpray ESI+ 5 kV 40 psi (275.8 kPa) 60 psi (413.7 kPa) 500 C
Flow: Instrument Detector Model #: Ion Source: Ion Mode: Ion Spray Voltage: Gas 1: Gas 2: Source Temp.:
4 10 2
5 1
0.0
1.0
2.0
3.0
4.0
5.0 Time (min.)
6.0
7.0
8.0
9.0
10.0
LC_EV0510
Carbamates in Orange Oil on Ultra Carbamate (LC-TOFMS)

Peak List: 1. aldicarb sulfone 2. aldicarb sulfoxide 3. oxamyl 4. methomyl 5. 3-hydroxycarbofuran 6. aldicarb 7. propoxur 8. carbofuran 9. carbaryl 10. methiocarb 11. BDMC (IS) Sample: Inj.: Conc.: Sample diluent: Matrix: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 531.1 Carbamate Pesticide Calibration Mix (cat.# 32273) and Internal Standard 4-bromo-3,5-dimethylphenyl-N-methylcarbamate (cat.# 32274) 50:50 spiked into unprocessed orange oil at 10ppm 3L 10ppm methanol orange oil Ultra Carbamate 9177352 50mm x 2.1mm 3m 100 A: 2mM ammonium acetate:methanol, 90:10 B: 2mM ammonium acetate:methanol, 10:90 Time (min.) %B 0 20 20 100 25 100 200L/min. ambient LECO Unique LC-TOFMS ESI Positive 130C 100kPa 4,000cc/min. 120C (+) 62V (+) 2.75kV
Flow: Temp.: Det.: Interface: Ion mode: Temp.: Nebulizer pressure: Desolvation gas (N2): Interface temperature: Nozzle: Capillary:
LC_FF0472
www.restek.com
719
Mar 2011
Food Contaminants
Pesticides on Pinnacle DB Aqueous C18 (LC/MS/MS, ESI+)
Sample: multicomponent pesticide standard Inj.: 5L Conc.: 33.3ppb each pesticide Sample diluent: acetonitrile Column: Cat.#: Dimensions: Particle size: Pore size: Pinnacle DB Aqueous C18 9418252 50mm x 2.1mm 1.9m 140 Compound fluometuron metobromuron flutriafol chlortoluron simetryn pirimicarb forchlorfenuron siduron ethofumesate cycluron diuron diethofencarb furalaxyl methiocarb secbumeton terbumeton prometon paclobutrazol promecarb dimoxystrobin ametryn methoprotryne triadimefon mexacarbate fludioxinil boscalid azoxystrobin methoxyfenozide cyproconazole prothioconazole flufenacet butafenacil myclobutanil dimethomorph bromuconazole 47 prometryn fipronil triticonazole tetraconazole uniconazole fluoxastrobin cyazofamid terbutryn tebufenozide chloroxuron picoxystrobin carfentrazone-ethyl diclobutrazol fenoxycarb diflubenzuron neburon flusiazole epoxiconazole fenbuconazole bupirimate zoxamide rotenone benalaxyl tebuconazole penconazole cyprodinil propiconazole alanycarb triflumuron thiobencarb pyraclostrobin benzoximate pinoxaden clofentezine trifloxystrobin prochloraz difenoconazole benfuracarb triflumizole buprofezin piperonyl butoxide pyriproxyfen propargite etoxazole amitraz noviflumuron pyridaben fenpyroximate fenpropimorph spiroxamine spinosyn A Polarity positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive negative negative positive positive positive negative positive positive positive positive positive positive negative positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive negative positive positive positive positive positive Mol. Wt. 232.21 259.1 301.3 212.68 213.31 238.29 247.68 232.32 286.35 198.31 233.1 267.33 301.34 225.31 225.29 225.29 225.29 293.8 207.27 326.39 227.33 271.39 293.75 222.28 248.19 343.21 403.3 368.47 291.78 344.26 363.34 474.82 288.78 387.86 377.06 241.36 437.15 317.81 372.12 291.78 458.83 324.78 241.36 352.47 290.75 367.25 412.17 328.21 301.34 310.67 275.18 315.4 329.76 336.82 316.41 336.54 394.42 325.41 307.82 284.19 225.29 342.22 399.52 358.68 257.78 387.83 363.8 400.52 303.15 408.38 376.67 406.28 410.53 345.75 305.44 338.45 321.28 350.48 359.42 293.41 529.1 364.94 421.5 303.49 297.48 731.97 RT (min.) 4.75 4.82 4.84 4.92 4.96 4.97 5.04 5.09 5.11 5.13 5.13 5.15 5.18 5.24 5.24 5.25 5.26 5.26 5.27 5.27 5.29 5.32 5.32 5.34 5.34 5.36 5.36 5.38 5.39 5.41 5.46 5.47 5.51 5.52, 5.54 5.54 5.55 5.56 5.58 5.6 5.62 5.62 5.63 5.65 5.65 5.67 5.67 5.69 5.71 5.72 5.72 5.74 5.76 5.76 5.76 5.77 5.77 5.79 5.83 5.84 5.93 5.96 5.96 5.98 5.99 6 6 6.01 6.01 6.11 6.12 6.21 6.29 6.29 6.38 6.4 6.42 6.52 6.68 6.87 6.89 7.08 7.18 7.2 7.38 7.63, 7.81 8.37 Transition 1 233.1 72.0 259.0 170.2 302.0 123.0 213.1 72.2 214.0 124.0 239.2 72.1 248.0 129.1 233.3 137.2 304.0 121.0 199.1 89.1 233.1 72.0 268.0 226.0 302.2 95.0 226.1 169.2 226.2 169.9 226.2 169.9 226.2 142.3 294.0 70.0 208.2 109.2 327.1 205.0 228.2 186.2 272.2 240.2 294.0 197.0 223.2 166.2 247.0 179.9 343.0 307 404.1 372.1 369.0 149.0 292.2 70.2 341.9 305.8 364.0 152.0 492.2 331.1 289.0 70.0 388.0 301.0 378.0 159.0 242.2 158.1 434.9 329.8 318.0 70.0 372.0 159.0 292.2 70.2 459.2 427.2 325.0 108.0 242.2 186.0 353.1 133.1 291.0 72.0 368.0 145.0 412.0 346.0 328.0 70.0 302.0 88.1 311.2 158.1 275.0 88.0 316.0 247.0 330.0 121.0 337.0 125.0 317.0 166.0 336.2 187.1 395.0 213.0 326.0 148.0 308.0 70.0 284.0 159.0 226.0 93.0 342.0 159.0 400.1 238.2 359.1 156.1 258.1 125.0 388.0 194.0 364.0 199.0 401.3 317.2 303.0 138.0 409.2 186.0 376.0 308.0 406.0 251.0 411.2 195.1 346.1 278.1 306.0 201.0 356.2 177.2 322.0 96.0 368.0 231.0 360.1 141.0 294.2 163.3 527.1 343.8 365.0 147.0 422.0 366.0 304.0 147.0 298.0 144.0 732.6 142.2
NEW!
LC_EV0479A
A: 10mM NH4OAc in water B: 10mM NH4OAc in methanol Time (min.) 0.0 1.0 8.0 10.0 11.0 %B 10 10 90 90 10
Flow: Temp.: Instrument: Det.:
600L/min. 35C Shimadzu Prominence UFLCXR Applied Biosystems 4000 QTRAP LC/MS/MS system Ion Source: TurboIonSpray, ESI+ IonSpray Voltage, ESI voltage: 5kV (ESI+) Gas 1: 40psi Gas 2: 60psi Source Temp.: 500C; max pressure ~7,200psi
Peak List: Compound methamidophos acephate bentazone omethoate bromoxynil butoxycarboxin aldicarb sulfoxide methomyl Ioxynil thiamethoxam monocrotophos dimethoate fenuron dioxacarb dicrotophos vamidothion carbendazim aldicarb formetanate acetamiprid carbetamide oxamyl aminocarb propoxur oxadixyl bendiocarb thiacloprid thiophanate methyl methabenzhiazuron tricyclazole pyracarbolid propamocarb carboxin ethiofencarb carbaryl thiabendazole carbanilide clethodim tebuthiuron
Polarity positive positive negative positive negative positive positive positive negative positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive positive
Mol. Wt. 141.13 183.17 240.28 213.14 276.91 222.27 206.26 162.21 370.92 291.7 223.17 229.26 164.21 223.23 237.19 287.34 191.19 190.27 221.26 222.67 236.27 219.26 208.26 209.24 278.31 223.23 252.71 342.4 221.28 189.23 217.27 188.27 235.3 225.31 201.22 201.25 212.25 359.91 228.32
RT (min.) 0.45 0.62 0.77 1.07 1.32 1.64 2.03 2.08 2.46 2.7 2.73 2.9 3.1 3.12 3.28 3.45 3.73 3.73 3.74 3.95 3.99 3.99 4.11, 4.44 4.15 4.21 4.24 4.25 4.3 4.31 4.35 4.38 4.41 4.51 4.52 4.58 4.6 4.6 4.61 4.68
Transition 1 142.0 94.0 184.0 142.8 239.0 131.8 214.0 124.9 275.9 80.8 223.1 86.1 207.1 132.1 163.1 88.1 369.8 126.7 292.0 211.0 224.1 127.0 230.1 199.0 165.1 72.1 224.0 123.0 238.0 112.0 288.0 146.0 192.0 160.0 208.1 116.0 222.1 165.2 223.1 126.1 237.0 192.0 237.1 72.2 209.2 137.1 210.1 111.0 279.0 219.0 224.1 109.1 253.2 126.1 343.0 151.0 222.0 165.1 190.0 163.0 218.2 125.0 189.2 102.2 236.0 143.0 226.1 106.9 202.1 145.1 202.0 175.0 213.1 94.0 360.0 164.0 229.2 172.4
720 www.restek.com
Food Contaminants
Pesticides on Ultra Aqueous C18 (LC/MS/MS)
NEW!
A: Pesticides in positive ion mode
Sample: Inj.: Conc.: Sample diluent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase:
multicomponent pesticide standard 10L 1ppb each pesticide acetonitrile Ultra Aqueous C18 9178312 100mm x 2.1mm 3m 100 Shimadzu Prominence UFLCXR A: 10 mM NH4OAc in water B: 10 mM NH4OAc in methanol Time (min.) 0.0 8.0 12.0 14.8 14.9 Flow: Temp.: %B 20 90 100 100 20 B: Pesticides in negative ion mode
0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0 14.0 15.0
Time (min.)
LC_FF0490
500L/min 35C
Det.: Ion Source: IonSpray Voltage: Gas 1: Gas 2: Source Temp.:
Applied Biosystems 4000 QTRAP LC/MS/MS system TurboIonSpray A & C: ESI+ B: ESI5kV (ESI+), -4.2kV (ESI-) 50psi 60psi 600C
0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 Time, min 8.0 9.0 10.0 11.0 12.0 13.0 14.0 15.0
LC_FF0490A
C: Improved retention of difficult pesticides in positive ion mode

omethoate
Visit www.restek.com/cat005 to view our "Comprehensive Pesticide Residue Analysis by LC/MS/MS Using an Ultra Aqueous C18 Column" article (contains compound identifications and MS details).
0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0 14.0
methamidophos acephate
for more info
propamocarb
Time (min.)
LC_FF0490B
www.restek.com
721
Mar 2011
Food Contaminants
Pesticides on Pinnacle DB Aqueous C18 (LC/MS/MS, ESI-)
NEW!
Peak List: Compound bentazone bromoxynil Ioxynil fludioxinil boscalid prothioconazole fipronil noviflumuron Polarity negative negative negative negative negative negative negative negative Mol. Wt. 240.28 276.91 370.92 248.19 343.21 344.26 437.15 529.1 RT (min.) 0.77 1.32 2.46 5.34 5.36 5.41 5.56 7.08 Transition 1 239.0 131.8 275.9 80.8 369.8 126.7 247.0 179.9 343.0 307 341.9 305.8 434.9 329.8 527.1 343.8 multicomponent pesticide standard Inj.: 5L Conc.: 33.3ppb each pesticide Sample diluent: acetonitrile Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Pinnacle DB Aqueous C18 9418252 50mm x 2.1mm 1.9m 140 A: 10 mM NH4OAc in water B: 10 mM NH4OAc in methanol Time (min.) 0.0 1.0 8.0 10.0 11.0 Flow: Temp.: Instrument: Det.: %B 10 10 90 90 10 Sample:
600L/min 35C Shimadzu Prominence UFLCXR Applied Biosystems 4000 QTRAP LC/MS/MS system Ion Source: TurboIonSpray, ESIIonSpray Voltage, ESI voltage: -4.2kV (ESI-) Gas 1: 40psi Gas 2: 60psi Source Temp.: 500C; max pressure ~7,200psi
LC_FF0479B
Sudan Dyes on Ultra Aqueous C18

Photodiode Array Detector Fixed Dual Wavelength Detector
wavelength change
1. 2. 3. 4.
Sudan I Sudan II Sudan III Sudan IV
Monitor Sudan I, II, III, and IV in a single, isocratic analysis!
LC_FF0326
LC_FF0327
Sample: Inj.: 20L, mixture of Sudan I, Sudan II, Sudan III, Sudan IV Conc.: 20g/mL each component Sample diluent: methanol Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Ultra Aqueous C18 9178565 150mm x 4.6mm 5m 100 methanol:water, 97:3 1mL/min. ambient UV @ 476/493/512/357nm (left) or UV @ 488/520nm (right)
722 www.restek.com
Drug Residues
Antibiotic Fluoroquinolones on Allure PFP Propyl
Peak List: 1. norfloxacin 2. levofloxacin 3. ciprofloxacin 4. lomefloxacin 5. enrofloxacin 6. sparfloxacin
Sample: Inj.: 5L Conc.: ~50g/mL each component Sample diluent: mobile phase Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Allure PFP Propyl 9169565 150mm x 4.6mm 5m 60 10mM potassium phosphate monobasic (pH 2.5): acetonitrile, 40:60 (v/v) 1.0mL/min. ambient UV @ 220nm
High organic (60% acetonitrile) means better LC/MS sensitivity!
Flow: Temp.: Det.:
LC_PH0420
Nonsteroidal Anti-inflammatory Drugs (NSAIDs) Ultra II Biphenyl

Sample: Inj.: 5L Conc.: 15g/mL each component Sample diluent: methanol Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Flow: Temp.: Det.: Ultra II Biphenyl 9609853 50mm x 3.0mm 2.2m 100 Shimadzu Prominence UFLCXR 20mM potassium phosphate, pH 2.5 with H3PO4:methanol (30:70) 1.2mL/min. 40C UV @ 254nm Peak List 1. ketoprofen 2. piroxicam 3. sulindac 4. diclofenac Ret. Time (min.) 0.894 1.068 1.197 1.465
NEW!
LC_PH0487
For more information on Biphenyl columns, visit
www.restek/biphenyl
www.restek.com
723
Mar 2011
Drug Residues
Nitrofuran Metabolites on Ultra C18 (LC/MS/MS)
d5-AMOZ
AMOZ
AHD
d4-AOZ
AOZ
SC
LC_0323
Peak List: 1. d5-AMOZ 2. AMOZ 3. AHD 4. d4-AOZ 5. AOZ 6. SC Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase:
Conc. (ppb) 0.3 0.3 0.3 0.3 0.3 0.3 Ultra C18 9174312 100mm x 2.1mm 3m 100
Time (min) 3.7 3.8 5.46 5.49 5.51 5.6
Analyzer Parameters: Ion source: ESI (electrospray ionization) Only segment: 15 min. Polarity: positive Data type: centroid Scan mode: SRM product Scan width (m/z): 0.7 Scan time (s): 0.25 Peak width: Q1: within 0.7 Q2: 0.7 Collision gas pressure (mTorr): 1.5 (argon) Divert valve: active, with 3 positions Positions-1 2 min., 2 8 min., 3 5 min. Analyte AOZ AMOZ SC AHD Prec. Ion 236 335 209 249 Prod. Ion 134 291 166 134 Collision E 12 V 10 V 12 V 12 V Tube Lens 120 100 80 110
Flow: Temp.: Det.:
A: 0.05% formic acid in methanol B: 0.05% formic acid 5 mM NH4 formate in water Time (min) %B 0 90 2.5 90 5 10 10 10 12 90 15 90 200L/min. 30C MS/MS triple quadrupoles (Thermo Scientific Discovery)
AMOZ = 3-amino-5-morpholinomethyl-2-oxazolidinone AHD = 1-aminohydantoin hydrochloride AOZ = 3-amino-2-oxazolidinone SC = semicarbazide
for more info

Visit www.restek.com/cat004 to view our "Analysis of Nitrofurans in Honey Using LC/MS/MS and an Ultra C18 Column" article.
724 www.restek.com
Drug Residues
Sulfonamides in Milk on Pinnacle DB Biphenyl (LC-TOFMS)
NEW!
milk spiked at 200ppb with sulfonamides, extracted with Q-sep Q110 QuEChERS extraction tube (cat.# 26213), and cleaned up with Q-sep Q211 QuEChERS dSPE clean-up tube (cat.# 26216), then concentrated. Inj.: 10L Conc.: 4g/mL Sample diluent: 0.2% formic acid Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Pinnacle DB Biphenyl 9409312 100mm x 2.1mm 3m 140 Compound 1. sulfadiazine 2. sulfathiazole 3. sulfamerazine 4. sulfamethazine 5. sulfamethoxypyridazine 6. sulfamethoxazole 7. sulfachloropyridazine 8. sulfadimethoxine 9. sulfaquinoxaline [M+H]+ 251 256 265 279 281 254 285 311 301 Sample:
Agilent 1100 with LECO Unique LC-TOFMS A: 0.2% formic acid B: methanol:acetonitrile (80:20), with 0.2% formic acid Time (min.) %B 0 15 20 100 30 100 Flow: 1mL/min. with preinjection split delivering 0.2mL/min. to column Temp.: ambient Det.: LECO Unique LC-TOFMS Interface: ESI Ion mode: positive Temp.: 120C Capillary: 3.8kV Cone: 50V Desolvation gas: 4L/min. Collected: 200-1,000 m/z
LC_FF0502
Sulfa Drugs Ultra II Biphenyl

Sample: Inj.: 3L Conc.: 25g/mL each component Sample diluent: methanol Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Ultra II Biphenyl 9609853 50mm x 3.0mm 2.2m 100 Shimadzu Prominence UFLCXR 0.1% formic acid in water:methanol (75:25) Time (min.) %B 0 25 3.5 65 1.0mL/min. 30C UV @ 254nm
Peak List Ret. Time (min.) 1. sulfadiazine 1.496 2 sulfathiazole 1.663 3. sulfamerazine 1.997 4. sulfamethoxazole 2.381 5. sulfamethazine 2.523 6. sulfachlorpyridizine 2.651 7. sulfamethoxine 3.228
NEW!
Flow: Temp.: Det.:
LC_PH0489
www.restek.com
725
Mar 2011
Preser vatives
Innovative food solutions at your fingertips!

Visit Resteks new website at
www.restek.com/fff
for all your testing needs.
Carboxylic Acids (Pyruvic and Lactic) on Ultra Aqueous C18

Peak List: 1. pyruvic acid 2. lactic acid Sample: Inj.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Conc. (mg/mL) 5 50 5L 50mM potassium phosphate, pH 2.5 Ultra Aqueous C18 9178565 150mm x 4.6mm 5m 100 50mM potassium phosphate, pH 2.5 1.0mL/min. 26C UV @ 210nm
Carboxylic Acids on Ultra Aqueous C18
restek innovation!
Excellent peak symmetry in 100% aqueous mobile phase!
Peak List: 1. malonic acid 2. lactic acid 3. acetic acid 4. citric acid 5. succinic acid 6. fumaric acid Sample: Inj.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 10L water
Conc. (g/mL): 500 500 1,000 1,000 2,000 10

1
5 3
Ultra Aqueous C18 9178565 150mm x 4.6mm 5m 100 50mM potassium phosphate, pH 2.5: acetonitrile (99:1) 1.5mL/min. 25C UV @ 210nm
2
4 min.
LC_0297
LC_0140
726 www.restek.com
Preser vatives, Sugars

Phenolic Antioxidants on Pinnacle II C18
Peak List: Conc. (ppm) 1. propyl gallate 168 2. TBHQ 182 3. 2-BHA + 3-BHA 197 4. BHT 193 Sample: Inj.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 10L methanol Pinnacle II C18 9214565 150mm x 4.6mm 5m 110 A: 1% acetic acid B: methanol Time B (min.) (%) 0 50 4 50 10 90 25 90 26 50 1.0mL/min. 30C UV @ 280nm
Flow: Temp.: Det.:
ChromaBLOGraphy
Topical and timely insights from top chromatographers.
Visit us at blog.restek.com
10
LC_0198
12
14
16
18 min.
Sugars on Pinnacle II Amino (3m)
Vanilla Bean Extract on Pinnacle DB C18 (Fast LC)

Sample: Inj.: Conc.: 5L 20% v/v commercial extract in water Pinnacle DB C18 9414555 50mm x 4.6mm 5m 140 0.2% v/v phosphoric acid in water:methanol (80:20 v/v) 2mL/min. 27C UV @ 254nm Peak List 1. vanillin Ret. Time (min.) 2.00
Peak List: 1. fructose 2. glucose 3. sucrose 4. maltose 5. lactose
Conc. (mg/mL) 2.0 2.1 4.0 4.5 4.4
Sample: Inj.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:
5L mobile phase Pinnacle II Amino 9217365 150mm x 4.6mm 3m 110 water:acetonitrile (25:75, v/v) 1.5mL/min. 35C refractive index @ 35C Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:
LC_0223
LC_0252
www.restek.com
727
Mar 2011
Flavor Compounds
Vanillin on Ultra C8
Sample: Inj.: Conc.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: 10mL 5% solution of vanilla extract 40% ethanol Ultra C8 9103565 150mm x 4.6mm 5m 100 Peak List: 1. vanillin
Vanillin and Ethyl Vanillin on Ultra C8

Peak List: 1. vanillin 2. ethyl vanillin Sample: Inj.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conc. (mg/mL) 0.12 0.04
10L 40% ethanol Ultra C8 9103565 150mm x 4.6mm 5m 100
Conditions: Mobile phases: A: 1.2% acetic acid in water B: methanol Time (min.) %B 0.0 20.0 5.0 20.0 15.0 40.0 20.0 40.0 25.0 20.0 Flow: 1.0mL/min. Temp.: 28C Det.: UV @ 254nm
Conditions: Mobile phases: A: 1.2% acetic acid B: methanol Time (min.) %B 0.0 20.0 5.0 20.0 15.0 40.0 20.0 40.0 25.0 20.0 Flow: 1.0mL/min. Temp.: 28C Det.: UV @ 254nm
8 LC_0149
10
12
14
16
18 min.
10
LC_0148
12
14
16
18 min.
Black Pepper: Piperine on Pinnacle II Cyano

Peak List: 1. piperine Sample: Inj.: Conc.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 5L 100g/mL methanol Pinnacle II Cyano 9216565 150mm x 4.6mm 5m 110
Capsaicinoids: Heat Level Assay for Habaero Nuggets on Pinnacle II C18

Peak List: 1. ethanol 2. unknown 3. capsaicin 4. dihydrocapsaicin Sample: Inj.: Conc.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 10L habaero nugget extract 0.8g sample in 200mL ethanol Pinnacle II C18 9214565 150mm x 4.6mm 5m 110 A: 1% acetic acid in water (v/v) B: acetonitrile Time (min.) % B 0 50 2 50 9 80 12 80 13 50 1.0mL/min. ambient UV @ 280nm
water:acetonitrile (50:50 v/v) 1.0mL/min. ambient UV/Vis @ 345nm
Flow: Temp.: Det.:
4
LC_0181
7 min.
LC_0160
728 www.restek.com
Dietar y Supplements
Melatonin Ultra II Aqueous C18
Peak List 1. melatonin Ret. Time (min.) 3.117
NEW!
Sample: Inj.: 1L Conc.: 100g/mL Sample diluent: water:methanol (60:40) Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Flow: Temp.: Det.: Pressure: Ultra II Aqueous C18 9608565 150mm x 4.6mm 5m 100 Shimadzu Prominence UFLCXR water:methanol (60:40) 2.0mL/min. 40C UV @ 222nm 240bar
LC_PH0506
Organic Acids Ultra II Aqueous C18
Peak List 1. tartaric acid 2. quinic acid 3. malic acid 4. citric acid 5. fumaric acid Sample: Inj.: Conc.:
Ret. Time (min.) 2.061 2.210 2.596 4.177 5.853
NEW!
5L 10g/mL fumaric acid, 2,000g/mL each other acids Sample diluent: water Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Flow: Temp.: Det.: Ultra II Aqueous C18 9608565 150mm x 4.6mm 5m 100 Shimadzu Prominence UFLCXR 100% 20mM potassium phosphate (pH2.5) 1.0mL/min. 30C UV @ 226nm
LC_PH0498
www.restek.com
729
Mar 2011
Dietar y Supplements
Allicin in Garlic Tablets on Pinnacle II C18
Peak List: 1. allicin Sample: Inj.: Conc.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 20L 1.2mg/mL garlic tablet in water deionized water Pinnacle II C18 9214565 150mm x 4.6mm 5m 110 water:methanol (50:50 v/v) 0.8mL/min. 30C UV @ 240nm
Phenethyl Glucosinolate on Ultra Aqueous C18
Peak List: 1. phenethyl glucosinolate
Sample: Inj.: Conc.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size:
10L 1,000g/mL water Ultra Aqueous C18 9178565 150mm x 4.6mm 5m 100
Conditions: Mobile phase: A: 50mM potassium phosphate, pH 2.5 B: acetonitrile Time (min.): % B 0.0 0 10 75 11 0 16 0 Flow: 1.0mL/min. Temp.: ambient Det.: UV @ 210nm
4
LC_0174
min.
LC_0166
Phenolics in Echinacea on Pinnacle II C18

Sample: Inj.: Conc.: Solvent: Sample temp.: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 10L 6.7mg/mL Echinacea capsule contents in sample diluent ethanol:water (70:30, v/v) 25C Pinnacle II C18 9214565 150mm x 4.6mm 5m 110 A: 0.1% phosphoric acid B: acetonitrile Time (min.) %B 0 10 13 22 14 40 14.5 40 15 10 20 10 1.5mL/min. 35C UV @ 330nm Peak List: 1. caftaric acid 2. chlorogenic acid 3. echinacoside 4. cichoric acid
Tocopherols in Soy Oil on Pinnacle II Silica

Peak List: 1. -tocopherol 2. -tocopherol 3. -tocopherol 4. -tocopherol Sample: Inj.: Conc.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size:
3
10L approx. 1.25% soy oil hexane Pinnacle II Silica 9210565 150mm x 4.6mm 5m 110 isopropyl alcohol:hexane (0.5:99.5) 0.6mL/min. 30C UV @ 295nm
Conditions: Mobile phase: Flow: Temp.: Det.:
Flow: Temp.: Det.:
4 1 2
0
LC_0195
8
LC_0197
10
12
14
min.
730 www.restek.com
Vitamins & Dietar y Supplements

Vitamin D on Ultra Aqueous C18 (LC/MS/MS)
Sample: Inj.: Conc.: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: 20L extracted serum sample Ultra Aqueous C18 9178352 50mm x 2.1mm 3m 100 Shimadzu Prominence UFLCXR A: 0.1% formic acid in water B: 0.1% formic acid in methanol Time (min.) %B 0.00 50 2.5 100 3.5 100 3.6 50 5.00 50 700L/min. 40C Applied Biosystems 3200 QTRAP LC/MS/MS system TurboIonSpray, APCI+ MRM 100msec. Q1 389.3 383.3 395.3 383.3 395.3 395.3 Q3 211.2 211.2 229.2 229.2 269.2 119.0 Declustering potential (V) 68 68 55 68 55 55 Ret. Time (min.) 3.00 3.00 3.04 3.00 3.04 3.04
NEW!
Flow: Temp.: Det.: Ion source: Mode: Dwell time: Compound d6-25-OH D3 (IS) 25-OH D3 25-OH D2 25-OH D3 25-OH D2 25-OH D2
LC_CF0492
for more info

Visit www.restek.com/cat003 to view our "5 Minute Analysis of Vitamin D in Serum by LC/MS/MS" article.
www.restek.com
731
Mar 2011

Vitamins (Fat Soluble) on Ultra C18
Peak List: Conc. (mg/mL) 1. solvent front n/a 2. menadione (vitamin K3) 0.45 3. all-trans-retinol (vitamin A) 0.34 4. vitamin D3 0.4 5. unknown n/a 6. tocopherol (vitamin E) 2.4 7. tocopherol acetate (vitamin E acetate) 2.4 8. unknown n/a 9. phylloquinone (vitamin K1) 0.84
Vitamins Thiamin (Vitamin B1) and Ascorbic Acid (Vitamin C) on Ultra IBD
Sample: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase:
diethyl ether Ultra C18 9174575 250mm x 4.6mm 5m 100 acetonitrile:methanol (90:10, v/v) Time (min.) Flow (mL/min.) 1.00 1.00 5.00 1.00 5.01 2.00 50.0 2.00 30C UV @ 280nm
Peak List: Conc. (mg/mL) 1. thiamin 2.5 2. ascorbic acid 2.5
Sample: Inj.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:
1.0L mobile phase Ultra IBD 9175565 150mm x 4.6mm 5m 100 50mM potassium phosphate, pH 2.5 1.0mL/min. ambient UV @ 254nm
Temp.: Det.:
3 6 7 9
1 5 8
10
20
LC_0144
30
40
min.
LC_0227
Restek is your Complete Source for
Analyzing Pesticides in Dietary Supplements

For more information on dietary supplements, visit
www.restek.com/dietary
732 www.restek.com

Fat Soluble Vitamins Ultra II C18
Peak List 1. vitamin K2 2. vitamin D2 3. vitamin D3 4. vitamin E acetate 5. vitamin K1 Ret. Time (min.) 0.905 1.224 1.305 1.828 2.169 Sample: Inj.: 1L Conc.: 100g/mL each component Sample diluent: acetone Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Flow: Temp.: Det.: Ultra II C18 9604853 50mm x 3.0mm 2.2m 100 Shimadzu Prominence UFLCXR acetonitrile:methanol (85:15) 1.5mL/min. ambient UV @ 230nm
NEW!
1 3
5 4
0.00
0.25
0.50
0.75
1.00
1.25 LC_PH0492
1.50
1.75
2.00
2.25
2.50
min.
Vitamins B1, B2, B3, and B6 Ultra C8

Peak List 1. vitamin B3 (nicotinamide) 2. vitamin B6 (pyridoxine) 3. vitamin B2 (riboflavin) 4. vitamin B1 (thiamine) Ret. Time (min.) 2.732 5.615 8.719 19.004
NEW!
Sample: Inj.: 5L Conc.: 50g/mL each component Sample diluent: water:methanol (80:20) Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Flow: Temp.: Det.: Ultra C8 9103575 250mm x 4.6mm 5m 100 Shimadzu Prominence UFLCXR 0.008M sodium 1-hexanesulfonate:methanol:glacial acetic acid: triethylamine (817.5:175:7.5:0.2) 2.0mL/min. 50C UV @ 270nm
LC_PH0497
www.restek.com
733
Mar 2011

Water Soluble B Vitamins Ultra II Aqueous C18
Sample: Inj.: 1L Conc.: 100g/mL each component Sample diluent: water:methanol (70:30) Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Ultra II Aqueous C18 9608565 150mm x 4.6mm 5m 100 Shimadzu Prominence UFLCXR A. 10mM potassium phosphate (pH 2.5) B. acetonitrile Time (min.) %B 0 2 1.5 2 5 75 1.5mL/min. 40C UV @ 210nm 105bar Peak List 1. vitamin B3 2. vitamin B6 3. vitamin B5 4. vitamin B9 5. vitamin B12 6. vitamin B2 7. vitamin B7 Ret. Time (min.) 2.472 2.764 3.804 4.126 4.261 4.329 4.472
NEW!
Flow: Temp.: Det.: Pressure:
LC_PH0503
Vitamin C Ultra II Aqueous C18
NEW!
Peak List Ret. Time (min.) 1. ascorbic acid (vitamin C) 1.759 Sample: Inj.: 2L Conc.: 100g/mL Sample diluent: water Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Flow: Temp.: Det.: Pressure: Ultra II Aqueous C18 9608565 150mm x 4.6mm 5m 100 Shimadzu Prominence UFLCXR 100% 10mM potassium phosphate (pH2.5) 1.5mL/min. 40C UV @ 242nm 95bar
LC_PH0504
734 www.restek.com

Vitamin A Compounds Ultra II Aromax
Peak List 1. retinol 2. -carotene Ret. Time (min.) 0.832 0.950
NEW!
Sample: Inj.: 2L Conc.: 100g/mL each component Sample diluent: acetone Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Flow: Temp.: Det.: Pressure: Ultra II Aromax 9607853 50mm x 3.0mm 2.2m 100 Shimadzu Prominence UFLCXR methanol:acetonitrile (99:1) 0.8mL/min. ambient UV @ 325nm and 480nm 105bar
UVat 325 (in red) UVat 480 (in black)
LC_PH0505

www.restek.com
735
Mar 2011
HPLC CHROMATOGRAMS | PHARMACEUTICAL
Famotidine
Famotidine and USP Impurities Ultra II Aromax
Sample: Inj.: Conc.: 10L 100g/mL famotidine, 10g/mL each impurity Sample diluent: methanol Column: Cat.#: Dimensions: Particle size: Pore size: Ret. Time (min.) 3.779 8.264 9.180 9.911 14.018 Conditions: Instrument: Mobile phase: Ultra II Aromax 9607565 150mm x 4.6mm 5m 100 Shimadzu Prominence UFLCXR 20mM potassium phosphate (pH 2.5):methanol Time (min.) %B 0 5 15 35 2.0mL/min. 40C 140bar UV @ 268nm
NEW!
Fast! 5m
Peak List 1. impurity A 2. famotidine 3. impurity D 4. impurity C 5. impurity B
Flow: Temp.: Pressure: Det.:
15 min.
LC_PH0495
Faster! 3m
Peak List 1. impurity A 2. famotidine 3. impurity D 4. impurity C 5. impurity B Ret. Time (min.) 2.094 4.460 4.937 5.334 7.480
Sample: Inj.: 5L Conc.: 100g/mL famotidine, 10g/mL each impurity Sample diluent: methanol Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Ultra II Aromax 9607313 100mm x 3.2mm 3m 100 Shimadzu Prominence UFLCXR 20mM potassium phosphate (pH 2.5):methanol Time (min.) %B 0 5 8 35 1.2mL/min. 40C 345bar UV @ 268nm
8 min.
LC_PH0494
Fastest! 2.2m
Peak List 1. impurity A 2. famotidine 3. impurity D 4. impurity C 5. impurity B Ret. Time (min.) 0.892 2.082 2.292 2.517 3.540
Sample: Inj.: 2L Conc.: 100g/mL famotidine, 10g/mL each impurity Sample diluent: methanol Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Ultra II Aromax 9607853 50mm x 3.0mm 2.2m 100 Shimadzu Prominence UFLCXR 20mM potassium phosphate (pH 2.5):methanol Time (min.) %B 0 5 4 35 1.2mL/min. 40C 480bar UV @ 268nm
4 min.
LC_PH0493
736 www.restek.com
Potential Genotoxic Impurities, Analgesics

Potential Genotoxic Impurities Ultra II Aromax
Peak List 1. ethyl benzenesulfonate 2. isopropyl toluenesulfonate 3. n-propyl toluenesulfonate 4. n-butyl toluenesulfonate *All M/Z are [M+NH4]+ M/Z* 204 232 232 246
NEW!
Sample: Inj.: 100L Conc.: 10ng/mL each PGI in 1mg/mL dorzolamide Sample diluent: mobile phase Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Flow: Temp.: Det.: Ultra II Aromax 9607312 100mm x 2.1mm 3m 100 Agilent 1100 A: 0.2% ammonium acetate in water B: 0.2% ammonium acetate in methanol 0.3mL/min. ambient LECO TOF-MS
LC_PH0482B
Hydroxybenzoic Acids on Ultra Aqueous C18
1. 2. 3. 4. 5. 6. 7.
3,5-dihydroxybenzoic acid 2,5-dihydroxybenzoic acid 4-hydroxybenzoic acid 3-hydroxybenzoic acid 2,4-dihydroxybenzoic acid benzoic acid salicylic acid
Sample: Inj.: 5L Conc.: 50g/mL each component Sample diluent: mobile phase Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Ultra Aqueous C18 9178565 150mm x 4.6mm 5m 100 A: 20mM potassium phosphate (pH 2.5); B: acetonitrile Time (min.) %B 0.00 20 5.00 50 10.00 50 1.0mL/min. ambient UV @ 210nm
Flow: Temp.: Det.:
LC_PH0400
www.restek.com
737
Mar 2011
Analgesics
Analgesic Acetaminophen and Narcotic Analgesics on Ultra C18
Peak List: Conc. (g/mL) U. unknown unknown 1. morphine sulfate 204 2. acetaminophen 92 3. codeine phosphate 216 4. oxycodone HCl 206 5. hydrocodone bitartrate 218
Narcotic Analgesic Morphine Sulfate Raw Material USP 25: Resolution Solution on Pinnacle II C18
Peak List: Conc. (g/mL) 1. unknown unknown 2. phenol 0.15 3. morphine sulfate 0.24 Sample: Inj.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 20L mobile phase Pinnacle II C18 9214575-700 250mm x 4.6mm 5m 110 A: 0.73g 1-heptane sulfonic acid and 10mL glacial acetic acid, diluted to 720mL with water, pH = 2.33 B: methanol (72A:28B, v/v) 1.00mL/min. 26.5C UV @ 284nm
Sample: Inj.: Sample: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size:
4.0L raw material mix mobile phase Ultra C18 9174575 250mm x 4.6mm 5m 100
Flow: Temp.: Det.:
A: 10mm potassium phosphate, pH 2.8 B: acetonitrile:methanol, (90:10, v/v) (85A:15B, v/v) 1.0mL/min. 35C UV @ 235nm
Flow: Temp.: Det.:
LC_0221
LC_0209
Narcotic Analgesic Hydrocodone Bitartrate by USP 25 on Pinnacle II Silica

Peak List: 1. hydrocodone bitartrate Sample: Inj.: Conc.: Sample: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 20L 1g/mL assay standard mobile phase Pinnacle II Silica 9210575 250mm x 4.6mm 5m 110 A: 800mL acetonitrile; 4mL water; 1mL diethylamine B: methanol (55A:45B, v/v) 1.5mL/min. 27C UV @ 280nm Ret. Time (min.) 3.1 Inj. % RSD (n = 5) 0.37%
Narcotic Analgesic Oxycodone HCl Raw Material by USP 25: Resolution Solution on Ultra C8
Peak List: Conc. (g/mL) 1. codeine phosphate 13 2. oxycodone HCl 9 Sample: Inj.: Sample: Solvent: 10L resolution solution mobile phase Ultra C8 9103564 150mm x 4.0mm 5m 100 A: 5mM hexane sulfonic acid with 2mL TEA and 3mL of phosphoric acid per liter. pH adjusted to 2.5 B: methanol (90A:10B, v/v) 1.5mL/min. 40C UV @ 206nm Ret. Time (min.) 19.3 26.8 RRT 0.7 1.0 Tailing 1.1 0.99 Res. 3.3
Flow: Temp.: Det.:
Impurities resolved from primary peak.
min.
LC_0211
LC_0213
738 www.restek.com
Antiarrhythmics, Antiasthmatics
Antiarrhythmic Calcium Channel Blockers on Ultra Cyano
Peak List: 1. diltiazem 2. nifedipine impurity 3. verapamil 4. nifedipine 5. nicardipine Sample: Inj.: Conc.: Solvent: 5L 100mg/mL acetonitrile:water (1:1) Ultra Cyano 9106565 150mm x 4.6mm 5m 100 20mM potassium phosphate monobasic, pH 3.0:acetonitrile (70:30, v/v) 1.2mL/min. 30C (1C) 235nm
Antiarrhythmic Furosemide on Ultra IBD
Peak List: 1. uracil (marker) 2. furosemide Sample: Inj.: Conc.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 5L 1000g/mL acetonitrile:water (60:40, v/v) Ultra IBD 9175565 150mm x 4.6mm 5m 100 20mM ammonium acetate, pH 4.5: acetonitrile (70:30, v/v) 2.0mL/min. 27C UV @ 280nm
1
Impurities in Furosemide
(enlargement of baseline)
Flow rate: Temp.: Det.:
4 5 3
5
LC_0062
9 min.
LC_0071
Antiasthmatic Beclomethasone on Ultra C18
Peak List: 1. beclomethasone 2. deschlorobeclomethasone Sample: Inj.: Conc.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:
1
10L 79.5g/mL (beclomethasone) water:acetonitrile (10:90, v/v) Ultra C18 9174565 150mm x 4.6mm 5m 100 water:acetonitrile (70:30, v/v) 1.0mL/min. 25C UV @ 238nm

10
LC_0120
15
20 min.
www.restek.com
739
Mar 2011
Antibiotics
Antibiotic Cephalexin on Ultra IBD
1 1
Antibiotic Penicillin V on Ultra IBD
Peak List: 1. cephalexin 2. cephradine Sample: Inj.: Conc.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 10L 500g/mL acetonitrile:water (10:90, v/v) Ultra IBD 9175565 150mm x 4.6mm 5m 100 10mM ammonium formate, pH 2.5: acetonitrile (90:10, v/v) 1.2mL/min. 30C UV @ 270nm
Peak List: 1. penicillin V Sample: Inj.: Conc.: Solvent:

2
2.5L 1.2mg/mL acetonitrile:water (10:90,v/v) Ultra IBD 9175565 150mm x 4.6mm 5m 100 10mM ammonium formate, pH 2.5: acetonitrile (95:5, v/v) 1.2mL/min. 30C UV @ 270nm
Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.:
0 0 2 4 6
LC_0094
min.
10 min.
LC_0096
Antibiotic Cephaloridine on Ultra IBD (Reversed Phase)
Tetracycline Mix on Allure Biphenyl

Peak List 1. oxytetracycline 2. degradation peak 3. tetracycline 4. degradation peak 5. chlortetracycline 6. doxycycline Ret. Time (min.) 4.59 5.19 6.32 11.16 15.81 19.66
Peak List: 1. cephaloridine Sample: Inj.: Conc.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 5L 1mg/mL acetonitrile:water (50:50, v/v) Ultra IBD 9175565 150mm x 4.6mm 5m 100 acetonitrile: 20mM ammonium phosphate, pH 4.0 (20:80, v/v) 1.2mL/min. 27C UV @ 254nm
Sample: Inj.: 30L Conc.: 100g/mL each component Sample diluent: methanol Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Allure Biphenyl 9166565 150mm x 4.6mm 5m 60 20mM ammonium phosphate (pH 2.5):acetonitrile, 80:20 1mL/min. ambient UV @ 254nm
5
LC_0102
min.
LC_PH0347
740 www.restek.com
Antibiotics, Anti-Diabetic, Cor ticosteroids

Antibiotic Amoxicillin on Ultra IBD Anti-Diabetic Glyburide (Glybenclamide) on Ultra IBD
2
Peak List: 1. amoxicillin Sample: Inj.: Conc.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.: 5L 1.5mg/mL acetonitrile:water (10:90, v/v) Ultra IBD 9175565 150mm x 4.6mm 5m 100 10mM ammonium formate, pH 2.5: acetonitrile (95:5, v/v) 1.2mL/min. 30C UV @ 270nm
Peak List: 1. unknown 2. glyburide Sample: Inj.: Conc.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.: 1L 500g/mL water:methanol:acetonitrile (1:1:2, v/v) Ultra IBD 9175565 150mm x 4.6mm 5m 100 water with 0.1% (v/v) acetic acid: acetonitrile (95:05, v/v) 1.0mL/min. 27C UV @ 254nm
min. 0 1 2 3
LC_0069
min.
LC_0095
Corticosteroids on Ultra C18

Peak List: 1. uracil (void marker) 2. triamcinolone 3. hydrocortisone 4. dexamethasone 5. corticosterone 6. deoxycorticosterone Sample: Inj.: Conc.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 5L 100g/mL mobile phase
5
Corticosteroids on Allure Biphenyl

Ret. Time (min.) 4.19 4.79 5.08 6.37 9.01 15.75 25.94
Peak List 1. hydrocortisone 2. prednisone 3. cortisone 4. dexamethasone 5. corticosterone 6. cortisone acetate 7. desoxycorticosterone
Sample: Inj.: 5L Conc.: 100g/mL each component Sample diluent: methanol Column: Cat.#: Dimensions: Particle size: Pore size:
6
Ultra C18 9174565 150mm x 4.6mm 5m 100 water:methanol (30:70, v/v) 1.0mL/min. 30C UV @ 220nm
Allure Biphenyl 9166565 150mm x 4.6mm 5m 60 water:acetonitrile, 60:40 1mL/min. ambient UV @ 254nm
2
LC_0108
6 min.
LC_PH0330
www.restek.com
741
Mar 2011
Steroids
Endogenous Steroids on Allure Biphenyl
Ret. Time (min.) 3.76 5.08 14.05
Contraceptive Hormones on Allure Biphenyl

Peak List 1. -estradiol 2. ethynyl estradiol 3. norethindrone 4. norgestrel Sample: Inj.: Conc.: Ret. Time (min.) 3.80 4.45 6.15 8.41
Peak List 1. -estradiol 2. testosterone 3. progesterone
Sample: Inj.: 5L Conc.: 100g/mL each component Sample diluent: methanol Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Allure Biphenyl 9166565 150mm x 4.6mm 5m 60 water:acetonitrile, 40:60 1mL/min. ambient UV @ 220nm
5L 100g/mL each component Sample diluent: methanol Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Allure Biphenyl 9166565 150mm x 4.6mm 5m 60 water:acetonitrile, 40:60 1mL/min. ambient UV @ 220nm
LC_PH0328 LC_PH0334
Hormones on 1.9m Pinnacle DB Biphenyl

Peak List: 1. estriol 2. 17-estradiol 3. 17-estradiol 4. ethynyl estradiol 5. testosterone 6. estrone 7. norethindrone
Get More!
Pharmaceutical Solutions Online
www.restek.com/pharma
LC_PH0453
Sample: Inj.: 1L Conc.: 100g/mL each component Sample diluent: water:methanol (50:50) Column: Cat.#: Dimensions: Particle size: Pore size: 1.9m Pinnacle DB Biphenyl 9409252 50mm x 2.1mm 1.9m 140
A: water B: methanol Time(min) %B 0 30 1 30 3 70 0.8 mL/min. 30C UV @ 220nm
Flow: Temp.: Det.:
742 www.restek.com
Lactulose Concentrate, Xanthines, Admixed Drugs

Laxative Lactulose Concentrate by USP 25: Resolution Solution on Pinnacle II Amino
Peak List: 1. fructose 2. galactose 3. epi-lactose 4. lactulose 5. lactose Conc. (mg/mL) 0.4 6.4 unknown 40 4.8 Ret. Time (min.) 4.6 6.1 10.0 10.5 12.7 RRT 0.44 0.58 0.95 1.00 1.21 Res. 1.1 2.9 Inj. % RSD (n = 5) 0.3%
Xanthines on Pinnacle DB C18

1 2
Sample: Inj.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size:
2L mobile phase Pinnacle DB C18 9414565 150mm x 4.6mm 5m 140
Sample: Inj.: 20L resolution standard Solvent: acetonitrile:water (50:50) Column: Cat.#: Dimensions: Particle size: Pore size: Pinnacle II Amino 9217365 150mm x 4.6mm 3m 110 Conditions: Mobile phase: Flow: Temp.: Det.: 10mM sodium phosphate monobasic in water, pH 4.8: acetonitrile (22:78, v/v) 1.3mL/min. 40C refractive index @ 40C
3 4
Conditions: Mobile phase: 20mM KH2PO4, pH 3.0: acetonitrile (90:10 v/v) Flow: 1.0mL/min. Temp.: 27C Det.: UV @ 254nm
min.
LC_0241
Peak List: Conc. (g/mL) 1. theobromine 225 2. theophylline 418 3. -hydroxyethyltheophylline 418 4. caffeine 400
LC_0222
Admixtures: Hydrocodone Bitartrate/Acetaminophen by USP 25 on Ultra C18

Peak List: Conc. (g/mL) 1. acetaminophen 0.76 2. hydrocodone bitartrate 0.0076 Ret. Time (min.) 3.304 6.664 RRT 1.0 2.0 Tailing Resolution Inj. % RSD (n = 5) 1.1 1.1 1.1 17.0 0.9
Admixtures: Expectorant/Antitussive Guaifenesin and Narcotic Analgesic Codeine on Ultra Phenyl

2 1
Sample: Inj.: Sample: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase:
25L 500mg acetaminophen with 5mg hydrocodone bitartrate (tablet) mobile phase Ultra C18 9174575 250mm x 4.6mm 5m 100 6.8g potassium monobasic with 0.2mL TEA per liter: acetonitrile (85:15, v/v) 1.5mL/min. 27C UV @ 210nm (hydrocodone bitartrate) and 295nm (acetaminophen).
Peak List: 1. codeine 2. guaifenesin Sample: Inj.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase:
Conc. (g/mL) 825 375 5L methanol:water (50:50) Ultra Phenyl 9105565 150mm x 4.6mm 5m 100 10mM ammonium formate, pH 2.5: acetonitrile (80:20, v/v) 1.2mL/min. 25C UV @ 280nm
Flow: Temp.: Det.:
0
LC_0212
min.
LC_0088
www.restek.com
743
Mar 2011
HPLC CHROMATOGRAMS | BIOCHEMICAL/CLINICAL
Nucleotides, Nucleosides, Nucleic Acid Bases

Nucleotides, Nucleosides, and Nitrogenous Bases on Ultra IBD
Peak List: Conc. (g/mL) 1. CDP 146 2. CMP 113 3. ATP 117 5 4. ADP 145 5. cytidine 155 6. TMP 157 7. AMP 125 8. guanine 36 9. guanosine 103 10. adenine 38 11. adenosine 115 Sample: Inj.: Solvent: 20L 20mM ammonium acetate, pH 5.8 Ultra IBD 9175565 150mm x 4.6mm 5m 100 20mM ammonium acetate, pH 5.8:methanol (97.5:2.5) 1.0mL/min. 35C UV @ 260nm
1 2 1 3 11 10 8 9
Uracil, Uridine, UTP, UDP, and UMP on Ultra IBD
Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:
5 2 4
Peak List: 1. UTP 2. UDP 3. UMP 4. uracil 5. uridine Sample: Inj.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:
Conc. (g/mL) 360 360 284 90 230
20L 20mM ammonium acetate, pH 5.8 Ultra IBD 9175565 150mm x 4.6mm 5m 100 20mM ammonium acetate, pH 5.8: methanol (97.5:2.5) 1.0mL/min. 35C UV @ 260nm
10
LC_0128
12
14
16
18
min.
4
LC_0133
6 min.
Thymine, Thymidine, TTP, TDP, and TMP on Ultra IBD
Nucleic Acid Bases on Allure PFP Propyl
Peak List: Conc. (g/mL) 1. TTP 224 2. TDP 152 3. TMP 346 4. thymine 88 5. thymidine 318 Sample: Inj.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 20L 20mM ammonium acetate, pH 5.8 Ultra IBD 9175565 150mm x 4.6mm 5m 100 20mM ammonium acetate, pH 5.8: methanol (97.5:2.5) 1.0mL/min. 35C UV @ 260nm
Peak List: 1. cytosine 2. uracil 3. guanine 4. thymine 5. adenine
Sample: Inj.: Conc. Solvent:
1.0L 100g/mL each 20 mM ammonium acetate, pH 5.0 Note: 1-3 drops of ammonium hydroxide added to keep guanine in solution Allure PFP Propyl 9169565 150mm x 4.6mm 5m 60 20mM ammonium acetate, pH 5.0: methanol (85:15, v/v) 1.0mL/min. ambient UV @ 260nm
4 5
2 3
Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:
4
10
LC_0132
12
14
16 min.
5
LC_0137
9 min.
744 www.restek.com
Catecholamines, Purines/Pyrimidines, Amino Acids, Peptides

Catecholamines on Allure PFP Propyl
Peak List Retention Time (min.) 1. norepinephrine 3.50 2. levodopa 5.43 3. epinephrine 7.27 4. tyrosine 7.77 5. dopamine 11.3 Sample: Inj.: Conc.: Sample diluent: Sample temp.: Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 10L 40g/mL each component mobile phase ambient Allure PFP Propyl 9169565 150mm x 4.6mm 5m 60 50mM ammonium phosphate (pH 3.0, adjusted with formic acid) 1mL/min. 35C UV @ 266nm
Purines/Pyrimidines on Ultra PFP

1
5 6 7 8
Peak List: 1. cytosine 2. 5-methylcytosine 3. uracil 4. uric acid 5. hypoxanthine 6. xanthine 7. thymine 8. purine 9. theobromine 10. ethyluracil 11. 6-methylpurine 12. 1,7-dimethylxanthine 13. theophylline 14. propyluracil Sample: Inj.: Conc.: Solvent:
11 12 13 14
9 4
10
10L 100g/mL each mobile phase
5 Column: Cat.#: Dimensions: Particle size: Pore size:
10
15
LC_0136
20
25 min.
Ultra PFP 9176575 250mm x 4.6mm 5m 100 0.001% formic acid in water: methanol (50:50, v/v) 1.0mL/min. ambient UV @ 260nm
LC_BA0349
Aromatic Amino Acids on Ultra Aqueous C18

Peak List: Conc. (mg/mL) 1. tyrosine 0.2 2. phenylalanine 1.6 3. tryptophan 0.4 Sample: Inj.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: 20L mobile phase A Ultra Aqueous C18 9178565 150mm x 4.6mm 5m 100
Peptide Mix on Viva C18

1. 2. 3. 4. 5. 6. 7.
mfr. H
val-tyr val-tyr-val meth enkephalin val-4-angiotensin III angiotensin II, III leucine enkephalin angiotensin I
*
mfr. D
Conditions: Mobile phases: A: 50mM potassium phosphate, pH 2.5 B: acetonitrile 5% - 20% B: 0-5 min. 20% - 5% B: 5-6 min. Hold at 5% B: 6-13 min. Flow: 1.0mL/min. Temp.: 30C Det.: UV @ 254nm
mfr. C
mfr. F 4 1
2
5 6 16.0 7 18.0 20.0 LC_BC0386
Viva 0.0 2.0 4.0 6.0 8.0
2 10.0 12.0
3 14.0
Sample: Inj.:
1
20L peptide test mix Viva C18 9514562 150mm x 2.1mm 5m 300
4
LC_0146
10
min.
A: 0.08% trifluoroacetic acid in water (pH 2.0) B: 0.08% TFA in acetonitrile, 10% B to 40% B in 20 min. Flow: 0.2mL/min. Det.: UV @ 214nm * High levels of trace metals (~100ppm) in the silica enhance this separation.
www.restek.com
745
Mar 2011
Proteins, Oxytocin
Protein Mix on Viva C18
Note excellent peak shapes and resolution on the Viva column!

Viva C18
(cat.# 9514562)
Manufacturer A
Peak List 1. ribonuclease A 2. cytochrome c 3. holo-transferrin 4. apomyoglobin
Ret. Time (min.) 11.31 14.65 16.32 20.34
Manufacturer B
Sample: Inj.: 20L Conc.: 0.08mg/mL each protein Sample diluent: 0.10% TFA in water / 0.10% TFA in acetonitrile, 80:20, v/v Sample temp.: 25C Columns: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Wide Pore C18 150mm x 2.1mm 5m 300 A: 0.10% TFA in water, B: 0.10% TFA in acetonitrile, 20% B to 70% B in 30 min. 0.20mL/min. 25C (or ambient) UV @ 214nm
Manufacturer C
Manufacturer D
Flow: Temp.: Det.:
LC_0324
PEGylated Oxytocin on Viva C18 (LC/MS)
free literature
Viva Wide Pore HPLC Columns Exceptional Performance for Peptides, Proteins, or Other Large Molecules Download your free copy from www.restek.com.
0.1% formic acid in water:0.1%formic acid in acetonitrile, 60:40 0.1mL/min. ambient Micromass Quattro II ESI positive 200C 2.25kV 40V
LC_PH0467
Sample: Inj.: Conc.: Sample diluent: Column: Cat.#: Dimensions: Particle size: Pore size:
oxytocin PEGylation reaction products 20L 300pmoles/L 0.1% formic acid in water (v:v) Viva C18 9514561 150mm x 1.0mm 5m 300
Conditions: Mobile phase: Flow: Temp.: Det.: Interface: Ion mode: Temp.: Capillary: Cone:
Flyer lit. cat.# 59939
746 www.restek.com
HPLC CHROMATOGRAMS | CLINICAL/FORENSIC
Pain Management Drugs

Pain Management Drugs in Urine on Ultra II Biphenyl (LC/MS/MS)
NEW!
Peaks RT (min.) 1. Acetaminophen 1.18 2. Morphine 1.79 3. Codeine 3.21 4. Oxycodone 3.46 5. Hydrocodone 3.60 6. Fentanyl 6.61 7. Buprenorphine 6.66 8. Lorazepam 6.79 9. Diazepam 8.06 10. Methadone 8.21 MRM1 152/110 286/157 300/165 316/298 300/199 337/132 468/187 321/275 285/154 310/77 MRM2 152/65 286/181 300/215 316/241 300/171 337/216 468/84 321/229 285/193 310/223
Recommended for opiates.
LC_CF0516
Column Dimensions: Particle Size: Pore Size: Temp.: Sample Conc.: Inj. Vol.: Mobile Phase
Ultra II Biphenyl (cat.# 9609352) 50 mm x 2.1 mm ID 3 m 100 40 C 5 ng/mL in 1:10 urine:mobile phase 5 L A: 0.1% formic acid in water B: 0.1% formic acid in methanol Time (min.) Flow (mL/min.) 0 0.5 10 0.5 10.1 0.5 12 0.5 %A 90 0 90 90 %B 10 100 10 10
Detector Model #: Ion Source: Ion Mode: Curtain Gas: Gas 1: Gas 2: Source Temp.: Source Voltage: Mode: Dwell Time: Instrument Acknowledgement
Applied Biosystems/MDS Sciex LC/MS/MS API-5000 TurboIonSpray ESI+ 25 psi (172.4 kPa) 60 psi (413.7 kPa) 40 psi (275.8 kPa) 550 C 2000 V MRM 50 ms Applied Biosystems/MDS Sciex LC/MS/MS System Special thanks to Applied Biosystems for providing instrument time.
www.restek/biphenyl
www.restek.com
747
Mar 2011
Opiates, THC
Opiates on Allure PFP Propyl (LC/MS/MS)
1. morphine 2. oxymorphone 3. hydromorphone 4. codeine 5. 6-monoacetylmorphine 6. oxycodone 7. hydrocodone
Conditions: Instrument: Mobile phase:
Shimadzu Prominence HPLC A: 0.1% formic acid in water B: 0.1% formic acid in 80:20, methanol:acetonitrile Time: 0.0 3.00 6.00 6.10 8.10 %B 10 50 50 10 Stop pumps
opiates 10L 25ug/mL methanol Allure PFP Propyl 9169552 50mm x 2.1mm 5m 60
Flow: Temp.: Det.: Ion source: IonSpray voltage: Gas 1: Gas 2: Source temp.:
0.40mL/min. 30C Applied Biosystems/MDS Sciex API 3200 MS/MS system Electrospray, positive 5,500 65psi (448kPa) 45psi (310kPa) 600C Mass Spectrometer Experiments: Declustering Collision Potential (V) Energy (V) 46 79 46 51 46 41 46 55 36 37 36 55 46 85 46 89 46 39 46 69 31 39 31 33 51 55 51 35
LC_PH0454
Compound morphine morphine hydromorphone hydromorphone oxymorphone oxymorphone codeine codeine hydrocodone hydrocodone oxycodone oxycodone 6-monoacetylmorphine 6-monoacetylmorphine
Q1 286 286 286 286 302 302 300 300 300 300 316 316 328 328
Q3 152 165 185 157 227 198 152 115 199 128 240 256 211 193
THC and Metabolites on Ultra II Biphenyl (LC/MS/MS)
NEW!
Column Dimensions: Particle Size: Pore Size: Temp.: Sample Diluent: Conc.: Inj. Vol.: Mobile Phase Peaks 1. Cannabidiol 2. THC-COOH-gluc 3. THC-COOH 4. Cannabinol 5. 9-THC MRM1 (Q1/Q3) 315/123 345/299 345/299 311/223 315/193 MRM2 (Q1/Q3) 315/193 345/193 345/193 311/178 315/123 Ultra II Biphenyl (cat.# 9609853) 50 mm x 3.0 mm ID 2.2 m 100 35 C Acetonitrile 50 ng/mL 20 L A: 0.1% formic acid in water B: 0.1% formic acid in methanol Time (min.) 0 0.50 3.50 4.50 4.60 6.00 Flow: Detector Model #: Ion Source: Ion Mode: Ion Spray Voltage: Curtain Gas: Gas 1: Gas 2: Source Temp.: Mode: Dwell Time: Instrument 0.7 mL/min. Applied Biosystems/MDS Sciex LC/MS/MS 3200 Q-Trap TurboIonSpray ESI+ 5 kV 25 psi (172.4 kPa) 50 psi (344.7 kPa) 60 psi (413.7 kPa) 550 C MRM 50 ms Applied Biosystems/MDS Sciex LC/MS/MS System %B 50 50 100 100 50 50
LC_CF0512
748 www.restek.com
Alcohol Metabolites, Diuretics

Alcohol Metabolites on Ultra II Biphenyl (LC/MS)
Sample: Inj.: 5L Conc.: 5g/mL each component Sample diluent: urine diluted 1:10 with mobile phase Column: Cat.#: Dimensions: Particle size: Pore size: Conditions: Instrument: Mobile phase: Ultra II Biphenyl 9609552 50mm x 2.1mm 5m 100 Shimadzu Prominence UFLCXR A: 5mM dihexylammonium acetate in water B: 5mM dihexylammonium acetate in methanol Time (min.) %B 0.0 40 2.5 40 2.6 100 5.4 100 5.5 40 7.5 40 0.3mL/min. 40C Shimadzu LCMS-2010EV ESISIM 200C -4,000V
NEW!
Peak List 1. matrix 2. ethyl glucuronide 3. ethyl sulfate
m/z 125 221 125
k' 2.75 4.02
Intensity 220,408 236,693
Flow: Temp.: Det.: Ion source: Mode: Source temp.: Source voltage:
LC_CF0500
Diuretics on Ultra II Biphenyl (LC/MS/MS, Negative Run)

MRM1 (Q1/Q3) 1. Acetazolamide 221/83 2. Chlorothiazide 294/214 3. Hydrochlorothiazide 296/78 4. Bendroflumethiazide 420/289 5. Furosemide 329/285 MRM2 (Q1/Q3) 221/80 294/179 296/269 420/328 329/205 MRM3 (Q1/Q3) 221/58 294/215 296/205 420/197 329/78
Diuretics in Urine on Ultra II Biphenyl (LC/MS/MS, Positive Run)

MRM1 (Q1/Q3) 1. Amiloride 230/171 2. Triamterene 254/237 3. Indapamine 366/132 4. Ethacrynic acid 303/179 5. Bumetanide 365/240 MRM2 (Q1/Q3) 230/116 254/104 366/91 303/194 365/156 MRM3 (Q1/Q3) 230/60 254/141 366/117 303/257 365/284
NEW!
Good retention for hydrophilic compounds!

Ion Mode: ESIIon Spray Voltage: -4.5 kV Ion Mode: ESI+ Ion Spray Voltage: 5.5 kV
LC_CF0510
LC_CF0509
Column Dimensions: Particle Size: Pore Size: Temp.: Sample Conc.: mobile phase Inj. Vol.:
Ultra II Biphenyl (cat.# 9609352) 50 mm x 2.1 mm ID 3 m 100 40C 500 ng/mL diuretics in urine, diluted 10x in 5 L
Mobile Phase A: 0.1% formic acid in water B: 0.1% formic acid in methanol Time (min.) Flow (mL/min.) 0 0.5 6.00 0.5 6.1 0.5 8.00 0.5 %A 90 0 90 90 %B 10 100 10 10
Detector Model #: Ion Source: Curtain Gas: Gas 1: Gas 2: Source Temp.: Mode: Dwell Time:
Applied Biosystems/MDS Sciex LC/MS/MS API 5000 TurboIonSpray 25 psi (172.4 kPa) 60 psi (413.7 kPa) 40 psi (275.8 kPa) 550C MRM 50 ms
www.restek.com
749
Mar 2011
Amphetamines, Cocaine
Amphetamines on Ultra II Biphenyl (LC/MS)
NEW!
Peaks 1. Amphetamine 2. Methamphetamine 3. MDA 4. MDMA 5. MDEA RT (min.) 2.812 3.432 3.537 4.092 4.679 m/z 135.95 149.95 179.95 193.95 207.95 Column Dimensions: Particle Size: Pore Size: Temp.: Sample Diluent: Conc.: Inj. Vol.: Mobile Phase Ultra II Biphenyl (cat.# 9609552) 50 mm x 2.1 mm ID 5 m 100 30 C mobile phase 2 g/mL 5 L A: 0.1% formic acid in water B: 0.1% formic acid in methanol Time (min.) Flow (mL/min.) 0 0.3 10 0.3 10.1 0.3 12.0 0.3 %A 80 5 80 80 %B 20 95 20 20
Detector Shimadzu 2010EV Acquisition Type: Scan Scan Speed: 2000 amu/sec. Heat Block: 200 C Interface: ESI+ Interface Temp.: 250 C Scan Range: 100 - 250 amu Event Time: 0.1 sec. Instrument Shimadzu UFLCXR Notes Data were collected in scan mode. An extracted ion chromatogram is shown.
LC_CF0518
www.restek/biphenyl
Cocaine and Ecgonine Methyl Ester on Allure PFP Propyl (LC/MS/MS)

Conditions: Mobile phase: 5mM ammonium formate, pH 3.0: acetonitrile (10:90, v/v) 0.6mL/min. ambient Applied Biosystems/MDS SCIEX API 3200 MS/MS system turbo ion spray, ESI 150C positive 5,000V + 71V + 265V nitrogen 2.2 mTorr 28 eV (COC) 26 eV (EME) 2,100 volts 7,000cc/min. 15lb/in.2 12lb/in.2
Peak List: 1. EME (ecgonine methyl ester) 2. COC (cocaine) Sample: Inj.: Conc.: Solvent: Temp.: Column: Cat.#: Dimensions: Particle size: Pore size: 10L 1g/mL water 4C Allure PFP Propyl 9169532 30mm x 2.1mm 5m 60
Flow: Column temp.: Det.: Interface: Interface temp.: Ion mode: ESI probe voltage: Orifice: Ring: Collision gas: Collision gas pressure: Collision gas energy: Electron multiplier: Auxilary gas flow: Nebulizer gas setting: Curtain gas setting:
1.30e3 cps
Get More!
Clinical, Forensic & Toxicology Solutions Online
www.restek.com/CFT
XIC of +MRM (3 pairs) for 200.0 / 182.0 amu
0.5
1.0
1.5
2.0
2.5
3.0
3.5
2
4.0
4.5
min.
XIC of +MRM (3 pairs) for 304.0 / 182.0 amu
2.35e3 cps
0 0.5 1.0 1.5 2.0 2.5 Data Courtesy of Shane Needham, Pfizer Inc.
3.0
3.5
4.0
4.5
LC_0126
min.
750 www.restek.com
Benzodiazepines
Benzodiazepines on Allure PFP Propyl (LC/MS/MS)
benzodiazepines 20L NA NA Allure PFP Propyl 9169552 50mm x 2.1mm 5m 60
Analyze 27 benzodiazepines in less than 10 minutes!
Conditions: Instrument: Shimadzu Prominence HPLC Mobile phase: A: 0.1% formic acid and 1mM ammonium formate in water B: 0.1% formic acid and 1mM ammonium formate in acetonitrile Time (min.) 0.0 10.00 15.00 15.50 17.50 Flow: Temp.: Det.: Ion Source: IonSpray Voltage: Gas 1: Gas 2: Source Temp.: Flow (L/min.) 500 1000 1000 500 500 %B 10 90 90 10 10
see gradient table 40C Applied Biosystems/MDS Sciex API 3200 MS/MS system Electrospray, positive NA NA NA 500C
Data courtesy of: Applied Biosystems MDS Sciex
LC_PH0463
MRM Transitions, retention times, and LOQ values.
Compound Name 7-aminonitrazepam 7-aminoclonazepam 7-aminoflunitrazepam Bromazepam -hydroxyalprazolam -hydroxytriazolam Oxazepam Lorazepam Estazolam Zaleplon 2-hydroxyethylflurazepam Desmethylflunitrazepam Nitrazepam Clonazepam Desalkylflurazepam Temazepam Triazolam Alprazolam Lormetazepam Clobazam Flunitrazepam Nordiazepam Zolpiclone D5-Diazepam Diazepam Chlordiazepoxide Prazepam Zolpidem Midazolam Flurazepam Medazepam D3-Doxepine
Bar color indicates shared precursor ions. Note compounds with shared precursor ions are baseline resolved on the Allure PFP Propyl column, as shown by retention time comparison.
Data courtesy of Applied Biosystems MDS Sciex.
Retention Time (min.) 3.2 3.3 3.8 3.8 4.1 4.1 4.2 4.3 4.4 4.4 4.5 4.5 4.6 4.7 4.7 4.7 4.7 4.8 4.8 4.9 5.0 5.0 5.4 5.4 5.5 6.0 6.1 7.4 7.9 8.5 9.0 9.1
Precursor Ion (amu) 252.1 286.1 284.1 316.0/318.0 325.1 359.0 287.0 321.0/323.1 295.0 306.2 333.1 300.1 282.0 316.0 289.1 301.1/303.1 343.0 309.1 335.0/337.1 301.1 314.0 271.1 389.1 290.1 285.0 300.1 325.1 308.1 326.1 388.2 271.0 283.0
MRM 1 (amu) 121.1 121.0 135.1 182.1 297.2 239.2 241.1 275.0 205.0 236.3 211.2 254.2 236.1 270.2 140.1 255.1 238.9 205.1 289.0 259.1 268.1 140.2 244.8 198.2 193.2 227.1 271.1 235.1 291.3 315.1 91.1 107.1
MRM 2 (amu) 94.0 222.2 226.0 182.1 204.9 176.0 268.9 277.0 267.1 264.2 109.0 198.2 180.2 214.0 226.1 257.2 314.9 281.1 291.1 224.3 239.1 164.9 217.0 154.1 283.2 140.0 236.1 222.0 317.1 207.3 -
DP 51 46 51 51 51 61 41 41 51 56 56 56 71 56 71 35 61 56 41 46 56 46 16 55 55 36 81 56 56 36 46 41
CE (MRM 1) 35 41 39 45 31 63 27 31 53 35 51 35 35 41 41 30 53 53 29 29 35 37 25 41 41 31 31 39 33 27 41 35
CE LOQ (MRM 2) (ng/mL) 53 1.0 35 0.5 49 0.5 45 5.0 59 2.0 37 5.0 19 10.0 27 5.0 31 2.0 27 0.5 41 1.0 51 2.0 51 2.0 51 2.0 39 2.0 30 5.0 37 1.0 35 1.0 29 2.0 47 1.0 49 1.0 35 2.0 41 1.0 37 1.0 21 5.0 53 2.0 35 0.2 63 0.5 27 0.1 39 2.0 -
www.restek.com
751
Mar 2011

Rtx11 12 - 708 751

Uploaded by

Document Information

Original Description:

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Rtx11 12 - 708 751

Uploaded by

Copyright:

Available Formats

HPLC CHROMATOGRAMS

HPLC Chromatograms by Column Phase Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .709 Environmental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .710-718

Foods & Flavors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .719-735

Website : www.chromtech.net.au E-mail : info@chromtech.net.au TelNo : 03 9762 2034 . . . in AUSTRALIA

HPLC Chromatograms by Column Phase

Allure Organic Acids

Allure PFP Propyl

Pinnacle DB Aqueous C18

GC & HPLC Chromatograms

Ultra II Aqueous C18

Ultra Aqueous C18

Chromatogram Search Tool

Website : www.chromtech.net.au E-mail : info@chromtech.net.au TelNo : 03 9762 2034 . . . in AUSTRALIA

HPLC CHROMATOGRAMS | ENVIRONMENTAL

Sample: Inj.: Conc.:

Flow: Temp.: Det.:

Aldehydes and Ketones (DNPH derivatives) on Ultra C18 (40C)

Flow rate: Det.: Temp.:

HPLC CHROMATOGRAMS | ENVIRONMENTAL

Explosives EPA Method 8330B Ultra C8

HMX RDX nitroglycerin nitrobenzene 4-amino-2,6-dinitrotoluene 3,5-dinitroaniline 2-nitrotoluene 2-amino-4,6-dinitrotoluene 3-nitrotoluene

10. 11. 12. 13. 14. 15. 16. 17.

PETN 4-nitrotoluene 1,3-dinitrobenzene 2,6-dinitrotoluene tetryl 2,4-dinitrotoluene 1,3,5-trinitrobenzene 2,4,6-trinitrotoluene

HPLC CHROMATOGRAMS | ENVIRONMENTAL

Flow: Temp.: Det.:

Herbicides on Allure C18

Flow: Temp.: Det.:

HPLC CHROMATOGRAMS | ENVIRONMENTAL

HPLC CHROMATOGRAMS | ENVIRONMENTAL

Flow: Temp.: Det.:

Phenoxyacid Herbicides on Allure Basix

Flow: Temp.: Det.:

HPLC CHROMATOGRAMS | ENVIRONMENTAL

Peak List: 1. diquat 2. paraquat

Peak time (min.) 7.5 8.8

Sample: Inj.: Conc.:

Paraquat and Diquat on Ultra Quat

Fast, sensitive LC/MS/MS analysis!

Peak List 1. diquat 2. paraquat

paraquat dichloride [CAS# 1910-42-5]

diquat dibromide [CAS # 85-00-7]

HPLC CHROMATOGRAMS | ENVIRONMENTAL

Flow: Temp.: Det.:

Diflubenzuron (Pesticide) on Ultra IBD

Jamie Hubler, Customer Service

Restek Customer Service

Outside the U.S.

HPLC CHROMATOGRAMS | ENVIRONMENTAL

Polycyclic Aromatic Hydrocarbons

Baseline resolution of PAHs in methanol!

Flow: Temp.: Det.:

Flow: Temp.: Det.:

HPLC CHROMATOGRAMS | ENVIRONMENTAL

Polycyclic Aromatic Hydrocarbons

Conditions: Mobile phase:

A: water B: acetonitrile Time (min.) %B 0 50 1 60 3 100 5 100 0.6mL/min. 30C UV @ 254nm

Flow: Temp.: Det.:

EU 256/2005 Polycyclic Aromatic Hydrocarbons on Pinnacle DB PAH

Conditions: Mobile phase:

A: water B: acetonitrile Time (min.) %B 0 50 1 90 2 95 5 100 7 100 0.6mL/min. 30C UV @ 254nm

Flow: Temp.: Det.:

HPLC CHROMATOGRAMS | FOODS & FLAVORS