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Symmetry®

ColumnsApplications

Notebook

Symmetry®

SymmetryShield™

Symmetry300™

SymmetryPrep™

Intelligent Speed (IS™)

1Waters, Symmetry, SymmetryShield, Sentry, SymmetryPrep, Platform LC, Quattro Ultima, IS, Oasis and Alliance are trademarks of Waters Corporation. ©2003 Waters Corporation.

Column: Symmetry® C18,4.6 x 150 mm, 5 µm

Mobile Phase A: H2OMobile Phase B: MeCNMobile Phase C: pH 3.75; 100 mM

NH4COOH in H2OFlow Rate: 1.4 mL/minIsocratic: 30% A; 60% B; 10% CInjection Volume: 5.0 µLTemperature: 30 °CDetection: UV @ 233 nm

Instrumentation: Waters Alliance® HT 2795Waters 996 PDA detectorSampling Rate: 5 pts./sec

Setting the Standard for Reproducibility

As today’s chemists establish new analytical methods for the latest pharmaceu-tical and biopharmaceutical products, theselection of a reproducible HPLC column isessential. The selected column needs to provide the same chromatographic resultsover the life of the new drug product.Symmetry® columns demonstrate superiorreproducibility over many years. Batches randomly selected over the past 5 yearsdemonstrate excellent reproducibility in theexample shown.

Reproducibility is our number one priority insupplying Symmetry® columns. This excellentreproducibility is a result of our commitmentto maintaining the tightest specifications in theHPLC column industry. Symmetry® columnsare engineered with high purity raw materials, tightly controlled manufacturingprocesses and column packing proceduresthat provide today’s scientists with the best,most reproducible HPLC column available.

Our goal is to supply a family of HPLCcolumns that you can rely on for rugged androbust methods. Symmetry® columns let youincrease your laboratorys' productivity, andallow easier method transfer between labsand around the globe.

A three-page Certificate of Analysis is included with every Symmetry® column. Wereport both our specifications, which are thetightest in the industry, and the results of the22 critical tests each column must passbefore it carries the Symmetry® brand.

RSD’s for Retention Times

1. Terbinafine HCl 0.7%

2. Ibuprofen 0.8%

3. Lovastatin 0.6%

4. Simvastatin 0.7%

Batch 136 (1998)

Batch 142 (1998)

Batch 149 (1999)

Batch 151 (2000)

Batch 156 (2001)

Unmatched Year-to-year Reproducibility

Comprehensive Certificate of Analysis

Minutes

Symmetry® Columns

2 Waters, Symmetry, SymmetryShield, Sentry, SymmetryPrep, Platform LC, Quattro Ultima, IS, Oasis and Alliance are trademarks of Waters Corporation. ©2003 Waters Corporation.

Table of Contents

Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

Compound Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-4

List of Applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8

Applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-182

Ordering Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .183-186

Notes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 187-192


Compound Index

Acephate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5, 9

Acetaminophen . . . . . . . . . . . . . . . . . . . . . . . 5, 11-13

Acetanilide . . . . . . . . . . . . . . . . . . . 122-123, 147-148

Acetophenone . . . . . . . . . . . . . . . . . . . . . . . . 147-148

2-Acetylfuran . . . . . . . . . . . . . . . . . . . . . . . . . 147-148

Acifluorfen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

Acyclovir . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5, 15-17

Alachlor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

Albuterol . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5, 18-19

Allobarbital . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33

Alpha-Tocopherol (Vitamin E) . . . . . . . . . . . . . . . . 179

6a-Methyl-17l-hydroxyprogesterone . . . . . . . . 122-123

2-Amino-7-chloro-5-oxo-5H-[1]

Benzopyrano[2,3-b]pyridine-3-carbonitrile . . . 122-123

7-Amino Clonazepam . . . . . . . . . . . . . . . . . . . . . . . 86

3-Aminofluoranthene . . . . . . . . . . . . . . . . . . . 122-123

7-Amino Flunitrazepam . . . . . . . . . . . . . . . . . . . . . . 86

7-Amino Nitrazepam . . . . . . . . . . . . . . . . . . . . . . . 86

Amitriptyline . . . . . . . . . . . . . . . . . . . . . . 173-175, 29

Amobarbital . . . . . . . . . . . . . . . . . . . . . . . . . . . 33-34

Amoxapine. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5, 21

Amoxicillin . . . . . . . . . . . . . . . . . . . . . . . . . . 5, 22-24

Amphetamine . . . . . . . . . . . . . . . . . . . . . . . . 5, 26-27

Ampicillin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5, 25

Angiotensin I . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115

Angiotensin II . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115

Antipyrine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5, 31

Atrazine . . . . . . . . . . . . . . . . . . . . . 5, 32, 36, 81, 172

AZT . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 182

β-hydroxyethyltheophylline (I.S.) . . . . . . . . . . . 45, 140

Bamethan (I.S.) . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

Barbital . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33

Beclomethasone . . . . . . . . . . . . . . . . . . . . . . 5, 35, 59

Benomyl . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5, 36, 81

Bentazon . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

Benzoic acid . . . . . . . . . . . . . . . . . . . . . . . . . 145-146

Benzophenone. . . . . . . . . . . . . . . . . . . . . . . . 147-148

Benzoylecgonine . . . . . . . . . . . . . . . . . . . . . . . . . . . 62

Betamethasone. . . . . . . . . . . . . . . . 5, 37-38, 149-150

Betamethasone Valerate . . . . . . . . . . . . . . . . . 149-150

Berberine. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

Bisphenol A . . . . . . . . . . . . . . . . . . . . . . . . . 5, 36, 81

2-Bromofluorene . . . . . . . . . . . . . . . . . . . . . . 122-123

8-Bromoguanosine . . . . . . . . . . . . . . . . . . . . . 122-123

BSA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39-42

Bupropion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5, 43

Busiperone . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5, 44

Butabarbital . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33-34

Butalbarbital . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33

Butalbital . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34

Butyl paraben . . . . . . . . . . . . . . . . . . . . 79, 135, 150

Butyrophenone . . . . . . . . . . . . . . . . . . . . . . . 147-148

Caffeine . . . . . . . . . . . . . . . . . . . . 5, 45, 48, 140, 170

Cafteric acid . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 125

Calcium Pantothenate . . . . . . . . . . . . . . . . . . . . . . 180

Captopril . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5, 46

Captopril Disulfide . . . . . . . . . . . . . . . . . . . . . . . . . 46

Carbadox. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5, 47

Catechins. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48

Carbamezapine . . . . . . . . . . . . . . . . . . . . . . . . . . . 30

Carbamezapine-10,11-epoxide . . . . . . . . . . . . . . . . 30

Carbaryl . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36, 81

Cefixime . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5, 49

Cefuroxime . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5, 50

Cephalexin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5, 51

Chloramben . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

Chloramphenicol . . . . . . . . . . . . . . . . . . . . . . . . . 5, 52

Chlorcyclizine HCL . . . . . . . . . . . . . . . . . . . . . . . . . 65

Chlordiazepoxide . . . . . . . . . . . . . . . . . . . . . 6, 53-54

2-Chloro-2,6-diethylacetanilide . . . . . . . . . . . . . . . . 10

Chlorogenic acid . . . . . . . . . . . . . . . . . . . . . . . . . . 125

Chlorpheniramine . . . . . . . . . . . . . . 6-7, 55, 137, 160

1-(3-Chlorophenyl)peperazine . . . . . . . . . . . . . . . . 171

Cholecalciferol (Vitamin D3) . . . . . . . . . . . . . . . . . 179

Cichoric acid . . . . . . . . . . . . . . . . . . . . . . . . . . . . 125

Cimetidine . . . . . . . . . . . . . . . . . . . . . . . . . . . 6, 56-58

Clavulanate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

Clobetasol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6, 59

Clonazepam . . . . . . . . . . . . . . . . . . . . . . . . . 6, 60, 86

Cocaethylene . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62

Cocaine . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6, 61-62

Codeine . . . . . . . . . . . . . . . . . . . . . 6, 11, 63-64, 139

Codeine-6-Glucuronide (C-6-G) . . . . . . . . . . . . . 63-64

Corticosterone . . . . . . . . . . . . . . . . . . . . . . . . 151-152

Cortisone . . . . . . . . . . . . . . . . . . . . . . . . . . . . 151-152

Cyanazine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172

Cyclizine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6, 65

Cytochrome C. . . . . . . . . . . . . . . . . . . . . . . . . 6, 66-69

2,4-D . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

2,4-DB . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

Demoxepam . . . . . . . . . . . . . . . . . . . . . . . . . . . 53-54

Deoxidized (Insulin). . . . . . . . . . . . . . . . . . . . . . . . . 91

Desamino (Insulin) . . . . . . . . . . . . . . . . . . . . . . . . . . 91

Desethylatrazine . . . . . . . . . . . . . . . . . . . . . . . 32, 172

Desethyldesisopropylatrazine . . . . . . . . . . . . . . . . . . 32

Desisopropylatrazine . . . . . . . . . . . . . . . . . . . . 32, 172

Dextromethorphan . . . . . . . . . . . . . . . . . . 6, 70-71, 87

Diazepam . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6, 72

Dicamba. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

3,5-Dichlorobenzoic Acid. . . . . . . . . . . . . . . . . . . . . 14

Dichlorprop . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

Diclofenac Sodium . . . . . . . . . . . . . . . . . . . . . . . 6, 73

2,6-Diethylaniline . . . . . . . . . . . . . . . . . . . . . . . . . . 10

10,11-Dihydrocarbamezapine . . . . . . . . . . . . . . . . . 30

Dihydroergotamine mesylate . . . . . . . . . . . . . . . . 6, 74

Dilitiazem HCL . . . . . . . . . . . . . . . . . . . . . . . . . . 75-76

Dinoseb . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

Diphenoxylate HCL . . . . . . . . . . . . . . . . . . . . . . . 6, 77

Diquat . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7, 120

Disopyramide . . . . . . . . . . . . . . . . . . . . . . . . . . . 6, 78

Doxepin . . . . . . . . . . . . . . . . . . . . 6, 29, 79, 173-175

Doxycycline . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 167

EDDP (Methadone Metabolite) . . . . . . . . . . . . . . . . . 99

Enalapril . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80

Ephedrine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26-27

Epicatechin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48

Epigallocatechin Gallate . . . . . . . . . . . . . . . . . . . . . 48

Estazolam . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99

Estradiol . . . . . . . . . . . . . . . . . . . . . . . . . . . . 151-152

Estrone . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 151-152

Ethosuximide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 153

Etodolac . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6, 83

Fenoprofen . . . . . . . . . . . . . . . . . . . . . . . . . . 131-132

Flunitrazepam . . . . . . . . . . . . . . . . . . . . . . . . 6, 85-86

Flurbiprofen . . . . . . . . . . . . . . . . . . . . . . . . . . 131-132

Folic Acid . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8, 181

Furazolidone . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 161

Furosemide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6, 88

Guanosine hydrate . . . . . . . . . . . . . . . . . . . . . . . . . 17

Heptanophenone . . . . . . . . . . . . . . . . . . . . . . 147-148

Hexanophenone . . . . . . . . . . . . . . . . . . . . . . 147-148

Hydrastine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

Hydrocodone Bitartrate . . . . . . . . . . . . . . . . . . . . 5, 12

Hydrocortisone . . . . . . . . . . . . . . . . . . 6, 89, 122-123

Hydrocortisone-21-Acetate . . . . . . . . . . . . . . . . . . . 89

4-Hydroxyantipyrine . . . . . . . . . . . . . . . . . . . . . . . . 31

Hydroxyatrazine . . . . . . . . . . . . . . . . . . . . . . . 32, 172

1-Hydroxybenzotriazole . . . . . . . . . . . . . . . . . . . . . 51

Hydroxydesethylatrazine . . . . . . . . . . . . . . . . . . . . . 32

Hydroxydesisopropylatrazine . . . . . . . . . . . . . . . . . . 32

7-(2-Hydroxyethyl) Theophylline . . . . . . . . . . . . . . 169

Ibuprofen . . . . . . . . . . . . . . . . . . . . . . 6, 90, 131-132

Imipramine . . . . . . . . . . . . . . . . . . . . . . . . . . 173, 175

Insulin(s) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91-93

Isorhamnetin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84

Kaempferol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84

Ketamine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 124

Ketoconazole . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94

Ketoprofen . . . . . . . . . . . . . . . . . . . . . . . . . . 131-132

Lasix (furosemide) . . . . . . . . . . . . . . . . . . . . . . . . . . 88

Click in the box, Type desired page number, Then click OK


Compound Index

Leu enkephalin . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82

Lidocaine HCL . . . . . . . . . . . . . . . . . . . . . . . . . . . 6, 95

Maleate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 160

Maleic Acid . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80

Maprotiline HCL . . . . . . . . . . . . . . . . . . . . . 6, 97, 171

MCPA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

MCPP . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

Meclizine HCL . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98

Mephenytoin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

Mephobarbital . . . . . . . . . . . . . . . . . . . . . . . . . 33-34

Met enkephalin . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82

Methadone . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7, 99

Methamphetamine . . . . . . . . . . . . . . . . . . . . . . . 26-27

Methoxyverapamil . . . . . . . . . . . . . . . . . . . . . 29, 178

Methsuximide . . . . . . . . . . . . . . . . . . . . . . . . . . . . 153

Methylparaben . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95

Methylphenidate HCL . . . . . . . . . . . . . . . . . . . . 7, 100

Metolachlor. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

Metolachlor-metabolite . . . . . . . . . . . . . . . . . . . . . . 10

Metoprolol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 134

Metoprolol tartrate . . . . . . . . . . . . . . . . . . . . . . 7, 101

Metronidazole . . . . . . . . . . . . . . . . . . . . . . 7, 102-103

Minocycline . . . . . . . . . . . . . . . . . . . . . . . . . . 167-168

Morphine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7, 104

Morphine-D3-glucuronide . . . . . . . . . . . . . . . . . . . 104

Morphine-D6-glucuronide . . . . . . . . . . . . . . . . . . . 104

N-Acetylprocainamide . . . . . . . . . . . . . . . . . . 128-129

N-Propionylprocainamide . . . . . . . . . . . . . . . 128-129

Nadolol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7, 105

Nalidixic acid. . . . . . . . . . . . . . . . . . . . . . . . 145, 161

Naloxone . . . . . . . . . . . . . . . . . . . . . . . . . . . . 106-109

Naltrexone . . . . . . . . . . . . . . . . . . . . 7, 106-109, 114

Naphtho(2,3-a)pyrene . . . . . . . . . . . . . . . . . . 122-123

Naproxen . . . . . . . . . . . . . . . . . . . . . . 7, 90, 110-111

Niacinamide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 180

Nicergoline . . . . . . . . . . . . . . . . . . . . . . . 7, 112, 181

Nifedipine . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7, 113

Nitrazepam . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86

4-Nitrophenol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

Norchlordiazepoxide . . . . . . . . . . . . . . . . . . . . . 53-54

Nordiazepam . . . . . . . . . . . . . . . . . . . . . . . . . . 53-54

Nordoxepin . . . . . . . . . . . . . . . . . . . . . . . 29, 174-175

Nortriptyline . . . . . . . . . . . . . . . . . . . . . . 29, 173-175

Norverapamil. . . . . . . . . . . . . . . . . . . . . . . 8, 29, 178

Octanophenone . . . . . . . . . . . . . . . . . . . . . . . 147-148

O-dichlorobenzene . . . . . . . . . . . . . . . . . . . . . . . . . 60

Oxazepam . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53-54

Oxolinic Acid . . . . . . . . . . . . . . . . . . . . . . . . . . . . 161

Oxprenolol . . . . . . . . . . . . . . . . . . . . . . . . . . 101, 134

Oxycodone . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7, 114

Oxytocin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7, 115

Paclitaxel (Taxol) . . . . . . . . . . . . . . . . . . . . 7, 116-117

Papaverine HCL . . . . . . . . . . . . . . . . . . . . . . . . . 7, 118

Paracetamol . . . . . . . . . . . . . . . . . . . . . . . . . . . 7, 119

Paraquat . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7, 120

Paraxanthine . . . . . . . . . . . . . . . . . . . . . . . . . 45, 140

Peptides. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7, 121

Perylene . . . . . . . . . . . . . . . . . . . . . . . . . . . . 122-123

Phencyclidine (PCP) . . . . . . . . . . . . . . . . . . . . . . . . 124

Phenobarbital . . . . . . . . . . . . . . . . . . . . 28, 30, 33-34

Phensuximide . . . . . . . . . . . . . . . . . . . . . . . . . . . . 153

2-Phenyl-2ethylmalonamide . . . . . . . . . . . . . . . . . . . 30

Phenytoin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30

Phthalic Acid . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 146

p-Hydroxyphenobarbital . . . . . . . . . . . . . . . . . . . . . 30

Picloram . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

Prednisolone . . . . . . . . . . . . . . . . . . . . . . . . . 149-152

Prednisolone Acetate . . . . . . . . . . . . . . . . . . . . . . . 149

Prednisone . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7, 126

Primidone . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28, 30

Procainamide . . . . . . . . . . . . . . . . . . . . . . 7, 127-129

Prochlorperazine Edisylate . . . . . . . . . . . . . . . . . . . 130

Progesterone . . . . . . . . . . . . . . . . . . . . . . . . . 151-152

Promethazine HCL . . . . . . . . . . . . . . . . . . . . . . . . . 133

Propiophenone . . . . . . . . . . . . . . . . . . . . . . . 147-148

Propranolol . . . . . . . . . . . . . . . . . . . . 7, 134-135, 160

Propylparaben . . . . . . . . . . . . . . . . . . . . . . . . . . 37-38

Protriptyline HCL . . . . . . . . . . . . . . . . . . . . . . . . . . 173

Pseudoephedrine HCL . . . . . . . . . . . . . . . . 7, 136-139

Pyridoxal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 180

Pyridoxamine Dihydrochloride . . . . . . . . . . . . . . . . 180

Pyrodoxine HCL . . . . . . . . . . . . . . . . . . . . . . . . . . 180

Quercetin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84

Quinidine sulfate . . . . . . . . . . . . . . . . . . . . . . . . 8, 141

Ranitidine . . . . . . . . . . . . . . . . . . . 8, 63-64, 142-144

Riboflavin . . . . . . . . . . . . . . . . . . . . . . . . . . . 180-181

Salbutamol . . . . . . . . . . . . . . . . . . . . . . . . . . 5, 18-19

Salicylic acid . . . . . . . . . . . . . . . . . . . . . . . 8, 145-146

Secobarbital . . . . . . . . . . . . . . . . . . . . . . . . . . . 33-34

Simazine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172

Succinimide . . . . . . . . . . . . . . . . . . . . . . . . 8, 28, 153

Succinylsulfathiazole . . . . . . . . . . . . . . . . . . . . 96, 154

Sulfadiazine . . . . . . . . . . . . . . . . . . . . . . 97, 154-157

Sulfadimethoxine . . . . . . . . . . . . . . . . . . . . . . 156-157

Sulfadimidine . . . . . . . . . . . . . . . . . . . . . . . . 156-157

Sulfamerazine . . . . . . . . . . . . . . . . . 97, 154-157, 159

Sulfamethazine . . . . . . . . . . . . . . . . . . . . . . . . 96, 154

Sulfamethoxazole . . . . . . . . . . . . . . . . . . . 8, 156-157

Sulfanilamide . . . . . . . . . . . . . . . . . 97, 127, 144, 154

Sulfathiazole . . . . . . . . . . . . . . . . . . . . . . 97, 154-157

Sulfisoxazole . . . . . . . . . . . . . . . . . . . . . . . . . 156-157

2,4,5-T . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

Tamoxifen citrate . . . . . . . . . . . . . . . . . . . . . . 162-163

Taxol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8, 116-117

Terconazole . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94

Terfenadine . . . . . . . . . . . . . . . . . . . . . . . . 8, 164-165

Testosterone acetate . . . . . . . . . . . . . . . . . . . . . . . . 166

Testosterone benzoate . . . . . . . . . . . . . . . . . . . . . . 166

Testosterone enanthate (I.S.) . . . . . . . . . . . . . . . . . . 166

Testosterone Propionate (I.S.) . . . . . . . . . . . . . . 35, 166

Tetracaine. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6, 87

Tetracycline. . . . . . . . . . . . . . . . . . . . . . . . . . . 167-168

Theobromine . . . . . . . . . . . . . . . . 8, 45, 140, 169-170

Theophylline . . . . . . . . 8, 45, 140, 147-148, 169-170

Thiamine Hydrochloride . . . . . . . . . . . . . . . . . 180-181

Toluamide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 160

2,4,5-TP . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

Trans-Retinol (Vitamin A) . . . . . . . . . . . . . . . . . . . . 179

Trazodone . . . . . . . . . . . . . . . . . . . . . . . 5, 8, 21, 171

Triamcinolone . . . . . . . . . . . . . . . . . . . . . . . . 122-123

Trimethoprim . . . . . . . . . . . . . . . . . . . . . . . 8, 158-159

Trimipramine . . . . . . . . . . . . . . . . . . . . . . . . 173, 175

Tripelennamine . . . . . . . . . . . . . . . . . . . . . . . . . 8, 176

Triprolidine HCL . . . . . . . . . . . . . . . . . . . . . . . 87, 138

Uracil . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 149, 179

Valerophenone . . . . . . . . . . . . . . . . . . . . . . . 147-148

Verapamil . . . . . . . . . . . . . . . . . . . . . . 8, 29, 177-178

Vitamins . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 179-181

Warfarin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6, 87

Zidovudine . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8, 182

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List of ApplicationsAcephate in Drinking Water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

Acetamide Herbicides and Metabolites in Drinking Water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

Acetaminophen and Codeine. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

Acetaminophen and Hydrocodone Bitartrate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12

Acetaminophen in Serum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13

Acidic Herbicides in Drinking Water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

Acyclovir . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15,16

Acyclovir in Plasma. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

Albuterol (Salbutamol) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18

Albuterol (Salbutamol) in Serum. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

Alkaloids in Golden Seal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

Amoxapine & Trazodone . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21

Amoxicillin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22

Amoxicillin & Clavulanate Potassium Augmentin Tablet . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

Amoxicillin in an Oral Suspension Formulation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

Ampicillin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

Amphetamines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26

Amphetamines in Human Urine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27

Anticonvulsants. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

Antidepressants in Plasma . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29

Antiepileptics & Metabolites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30

Antipyrine & Its Metabolites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31

Atrazine & Metabolites in Drinking Water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32

Barbiturates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33

Barbiturates in Human Urine. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34

Beclomethasone. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35

Benomyl & Bisphenol A. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36

Betamethasone. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37

Betamethasone in Syrup Formulation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38

BSA Tryptic Digest . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39

BSA Tryptic Digest - Column Length Effects . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40

BSA Tryptic Digest - Flow Rate Effects . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41

BSA Tryptic Digest - Gradient Duration Effects . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42

Bupropion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43

Busiperone . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44

Caffeine and Metabolites in Serum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45

Captopril . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46

Carbadox. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47

Catechins - 4.6 x 20 mm Intelligent Speed™ Separation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48

Cefixime. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49

Cefuroxime . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50

Cephalexin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51

Chloramphenicol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52


Click on the application titles below to go directly to the desired applicationFor a new search, click on the "List of Applications" bookmarks to the left


List of ApplicationsChlordiazepoxide & Metabolites. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53

Chlordiazepoxide & Metabolites in Serum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54

Chlorpheniramine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55

Cimetidine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56-58

Clobetasol and Related Compound . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59

Clonazepam . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60

Cocaine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61

Cocaine & Its Metabolites in Serum. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62

Codeine and Its Glucuronide Metabolite in Human Urine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63

Codeine and Its Glucuronide Metabolite in Porcine Plasma . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64

Cyclizine & Chlorcyclizine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65

Cytochrome c Tryptic Digest - Column Lifetime Study, Critical Pair Resolution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66

Cytochrome c Tryptic Digest - Pore Size Effects . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67

Cytochrome c Tryptic Digest - Recovery Study . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68

Cytochrome c Tryptic Digest - Reproducibility Study . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69

Dextromethorphan . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70

Dextromethorphan in a Cough Syrup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71

Diazepam in Serum - LC/MS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72

Diclofenac Sodium . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73

Dihydroergotamine Mesylate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74

Diltiazem HCL . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75

Diltiazem HCL -Isolation of Impurities, Transfer from Analytical to Prep . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 76

Diphenoxylate HCL. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77

Disopyramide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 78

Doxepin in Serum. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 79

Enalapril . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80

Endocrine Disruptors in Soil . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81

Enkephalins . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82

Etodolac . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83

Flavanoids in Ginko . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84

Flunitrazepam . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85

Flunitrazepam and Related Compounds . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86

Four Drug Mixture: Warfarin, Dextromethorphan, Triprolidine, and Tetracaine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 87

Furosemide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 88

Hydrocortisone and Related Compunds. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89

Ibuprofen and Naproxen in Serum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 90

Insulin Chain - QC Batch Test for Symmetry 300™. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91

Insulin- Impurity Isolation, Transfer from Analytical to Prep . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92

Insulin- Isophase Suspension . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93

Ketoconazole. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94

Lidocaine HCL . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95

Lifetime of 3.5 µm Symmetry® Column: 10,000 Injections of Sulfa Drugs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96

Maprotiline HCL. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97


List of ApplicationsMeclizine HCL. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98

Methadone in Human Urine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99

Methylphenidate HCL . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100

Metoprolol Tartrate and Oxyprenolol. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101

Metronidazole . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 102,103

Morphine & Its Glucuronide Metabolites in Serum. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 104

Nadolol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 105

Naltrexone . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 106

Naltrexone in Plasma . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 107

Naltrexone in Plasma - LC/MS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 108

Naltrexone in Serum. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109

Naproxen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 110,111

Nicergoline . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 112

Nifedipine. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 113

Oxycodone in Serum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 114

Oxytocin & Angiotensins in Serum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115

Paclitaxel (Taxol) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 116

Paclitaxel (Taxol)- Resolution of Impurities. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117

Papaverine HCL. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 118

Paracetamol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119

Paraquat & Diquat in Tap Water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 120

Peptides- Alberta Peptide Mixture . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 121

Pharmaceutical Test Mix - 2.1 x 20 mm Intelligent Speed™ Separation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 122

Pharmaceutical Test Mix - 4.6 x 20 mm Intelligent Speed™ Separation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 123

Phencyclidine in Human Urine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 124

Phenolics in Echinacea . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 125

Prednisone. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 126

Procainamide in Serum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 127

Procainamides at pH 3.0 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 128

Procainamides at pH 6.0 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 129

Prochlorperazine- Isolation of Degradation Products, Transfer from Analytical to Prep . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 130

Profens (Gradient) - 4.6 x 20 mm Intelligent Speed™ Separation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 131

Profens (Isocratic) - 4.6 x 20 mm Intelligent Speed™ Separation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 132

Promethazine- Impurities Profile . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 133

Propranolol in Human Urine. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 134

Propranolol in Serum. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 135

Pseudoephedrine HCL. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 136

Pseudoephedrine HCL & Chlorpheniramine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 137

Pseudoephedrine HCL & Triprolidine HCL . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 138

Pseudoephedrine HCL & Codeine. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 139

Purine Alkaloids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 140

Quinidine Sulfate and Related Substance. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 141

Ranitidine. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 142,143




List of ApplicationsRanitidine in Serum. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 144

Salicyclic Acid & Related Compounds in Serum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 145

Salicyclic Acid & Related Compounds. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 146

Speed Mix - 2.1 x 20 mm Intelligent Speed™ Separation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 147

Speed Mix - 4.6 x 20 mm Intelligent Speed™ Separation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 148

Steroids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 149

Steroids in Serum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 150

Steroids - 2.1 x 20 mm Intelligent Speed™ Separation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 151

Steroids - 4.6 x 20 mm Intelligent Speed™ Separation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 152

Succinimides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 153

Sulfa Drugs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 154,155

Sulfa Drugs - 2.1 x 20 mm Intelligent Speed™ Separation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 156

Sulfa Drugs - 4.6 x 20 mm Intelligent Speed™ Separation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 157

Sulfamethoxazole Oral Suspension . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 158

Sulfamethoxazole and Trimethorprim in Serum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 159

Symmetry® C18 pH 3 Batch Test. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 160

Synthetic Antibiotics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 161

Tamoxifen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 162

Tamoxifen, Isolation of Impurities, Transfer from Analytical to Prep Columns . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 163

Terfenadine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 164

Terfenadine and Related Compound. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 165

Testosterone Esters in Serum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 166

Tetracyclines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 167

Tetracyclines in Serum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 168

Theophylline & Related Compounds . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 169

Theophylline & Theobromine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 170

Trazodone. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 171

Triazine Herbacides in Drinking Water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172

Trycyclic Antidepressants . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 173

Trycyclic Antidepressants & Metabolites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 174

Trycyclic Antidepressants in Plasma . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 175

Tripelennamine. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 176

Verapamil . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 177

Verapamil and Norverapamil. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 178

Vitamins: Fat-Soluble . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 179

Vitamins: Water-Soluble. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 180

Vitamins: Water-Soluble Folic Acid Mixture. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 181

Zidovudine (AZT) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 182


Acephate in Drinking Water

acephate

Minutes0 10 155

blank cartridge

nonspiked sample

spiked tap water

Oasis® HLB Extraction MethodConditions for Oasis® HLB Cartridge, 3 cc, 60 mg

Part Number WAT094226

% RecoverySpike Level Spike Level10 µg/L 5 µg/L5 replicates 7 replicates91.0% (16.3% RSD) 83.6% (15.0% RSD)

(Source water: chlorinated municipal tap water)

HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µmPart Number: WAT200655Mobile Phase: H2O/ACN 96:4Flow Rate: 1.0 mL/minInjection volume: 75 µLDetection: UV @ 200 nm (0.02 AUFS)

SP

NC

O

CH3

OH3C

HOH3C

- contact and systematic organophosphorous insecticide- highly polar, water soluble

Prepare Sample:To 20 mL sample add 5 g NaCl

Adjust to pH 3 with H3PO4

Condition:3 mL methylene chloride

Rinse: 3 mL methanolRinse: 3 mL H2O

Load:20 mL sample @ 4 mL/min

Elute:2 mL methylene chloride

Evaporate and Reconstitute:with 250 µL mobile phase

Acephate


Minutes


Acetamide Herbicides and Metabolitesin Drinking Water

Minutes0 10 20

1

2 3 4 5

spiked well water(200 ng/L)

blank cartridge

nonspiked sample



Compounds % RecoveryTap Water Tap Water Well Water2.0 µg/L 200 ng/L 200 ng/L5 replicates 5 replicates 5 replicates

1. Metolachlor-metabolite* 99.1 (10) 78.9 (22) 88.3 (3.3)2. 2-Chloro-2,6-diethylacetanilide 98.5 (3.8) 109 (34) 105 (24)3. 2,6-Diethylaniline 93.3 (11) 80.3 (23) 89.2 (7.8)4. Alachlor 93.9 (3.2) 90.1 (21) 89.9 (1.2)5. Metolachlor 97.1 (6.6) 93.0 (16) 112 (3.3)

* 2-[(2-ethyl-6-methylphenyl)amino]1-propanol

HPLC Method

Column: Symmetry® C8 3.9 x 150mm, 5µm Part Number: WAT046970Mobile Phase A: 10mm phosphate buffer pH 6.8,/acetonitrile 70:30Mobile Phase B: AcetonitrileGradient: Time Profile

(min) %A %B0 100 020 40 60

Flow Rate: 1.2 mL/minInjection volume: 80 µLDetection: UV @ 214 nm (0.02 AUFS)

CH2CH3

CH2CH3

N

COCH2Cl

CH2OCH3

Condition:3 mL methanol

Rinse:2 mL H2O


Wash:1 mL H2O

Elute:1.2 mL methanol

Evaporate to 0.2 mLReconstitute to 0.5 ml with reagent H2O

Alachlor

Minutes


Acetaminophen and Codeine

HPLC Method

Column: Symmetry® C8, 3.9 x 150mm, 5 µmPart Number: WAT046970Mobile phase: 10mM docusate sodium in methanol/water/THF/phosphoric acid 60:36:4:1Flow rate: 0.75mL/minInjection volume: 15 µL of 55µg/mL acetaminophen and 35 µg of codeine sampleDetection: UV @ 254 nm

USP Tailing Factors

1. 1.092. 1.04

1

2

0 2 4 6 8 10 12

Minutes

1. Acetaminophen

2. Codeine

Minutes


Acetaminophen and Hydrocodone Bitartrate

HPLC Method

Column: Symmetry® C18, 3.9 x 150mm, 5µmPart Number: WAT046980Mobile phase: 50 mM Ammonium phosphate, pH 5.8/acetonitrile 85:15 Flow rate: 1.0 mL/minInjection volume: 20 µL of 775µg/mL acetaminophen and 8 µg hydrocodone bitartrate sampleDetection: UV @ 214 nm

1. Acetaminophen

2. Hydrocodone Bitartrate

Minutes


Acetaminophen in Serum

0.02 AU

1

2

B

A

0 4 8 12Minutes

Oasis® HLB Extraction MethodOasis® HLB 1 cc/30 mg Extraction Cartridge


Compound Concentration % Recovery %RSD µg/mL (n=6)

Acetaminophen 0.100 107% 1.5%

0.500 101% 0.40%

HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ guard column, 3.9 x 20 mm, 5 µmPart Numbers: Column - WAT200655, Guard - WAT200675Mobile phase: 20 mM potassium phosphate, pH 3.0/methanol 97:3)Flow rate: 1.0 mL/minInjection volume: 50 µL of reconstituted porcine serum extractTemperature: 30˚ CDetection: UV @ 220 nm

Compounds:1: Sulfanilamide (I.S.)2: Acetaminophen

HO

O

2CHHN

Condition1 mL methanol/1 mL water

Load1 mL spiked porcine serum

Wash1 mL 5% methanol in water

Elute1 mL methanol

Evaporate and Reconstitute40 ˚C under nitrogen stream

200 µL of 50 µg/mL sulfanilamide(I.S.) in water

2. Acetaminophen

Chromatogram of Serum Extracts: A) Blank B) Spiked Sample

Minutes

1. Sulfanilamide (I.S)


Acidic Herbicides in Drinking Water

15

Minutes0 10 20 30

1

23

4 5

67 8

91011 12

1314

spiked tap water(400 ng/L)

nonspiked sample

Compounds

1. Picloram2. Dicamba3. Chloramben4. 4-Nitrophenol5. Bentazon6. 2,4-D

7. MCPA8. Dichlorprop9. 2,4,5-T

10. MCPP11. 3,5-Dichlorobenzoic12. 2,4-DB

13. 2,4,5-TP

14. Acifluorfen15. Dinoseb

HPLC Method

Column: SymmetryShield™ RP8 3.9 x 150mm, 5µmPart Number: WAT200655Mobile Phase A: 13 mM phosphate buffer, pH 3.4Mobile Phase B: AcetonitrileGradient: Time Profile

(min) %A %B0 85 158 70 3015 70 3030 40 6035 10 90




Prepare Sample: 75 mL sample,adjust to pH 2 with H3PO4

Condition:3 mL 10:90 methanol/MTBE*

Risnse: 2 mL methanolRinse: 2 mL H2O


Wash:1 mL H2O

Elute:2 mL 10:90 methanol/MTBE*

Evaporate to 0.2 mLReconstitute to 0.5 mL with H2O

* methyl t-butyl etherdiethyl ether can be used as an alternative to MTBE

N

Cl

OH

O

N

Cl

Cl

1. Picloram

Cl

OH

O

N

Cl

3. Chloramben

N+

O O

OH

4. 4-Nitrophenol

N

S

N

O

O

O

9. 2,4,5-T5. Bentazon

O

Cl

Cl

OH

O

6. 2,4-D

O

Cl

OH

O

7. MCPA

Cl

OHO

Cl

11. 3,5-Dichlorobenzoic acid

O

Cl

Cl

OH

O

8. Dichloroprop

O

Cl

OH

O

10. MCPP

OO

N+

O

O

O

F

F

F

Cl

O OO

N

14. Acifluorfen

OH

N+

N+

O

O

O O

15. Dinoseb

O

Cl

Cl

Cl

OH

O

13. 2,4,5-TP

O

Cl

Cl

OH

O

12. 2,4-DB

2. Dicamba

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µmPart number: WAT046970Mobile phase: 0.1% glacial acetic acid (aq), pH 3.3Flow rate: 1.0 mL/minInjection volume: 5 µL of 100 µg/mL sampleDetection: UV @ 254 nm

USP Tailing Factors

1. 1.1

Minutes

Acyclovir

1. Acyclovir


HPLC Method

Column: SymmetryShield™ RP18, 4.6 x 150 mm, 5 µmPart number: 186000109Mobile phase: 20 mM, pH 7.0 phosphate buffer/acetonitrile 95:5Flow rate: 1.0 mL/minInjection volume: 5 µLDetection: UV @ 254 nm

USP Tailing Factors

1. 1.1

Acyclovir

1. Acyclovir

Minutes


Acyclovir in Plasma


Acyclovir 1.0 95.1% 3.4%0.20 98.3% 5.0%

HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ guard column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT200655, Guard - WAT200675Mobile phase: 20 mM ammonium acetate, pH 5Flow rate: 1.0 mL/minInjection volume: 50 µLDetection: UV @ 250 nm

Compounds:1. Acyclovir2. Guanosine hydrate

Chromatogram of Plasma Extracts: A) Blank B) Spiked Sample

2. Guanosine hydrate (I.S.)



Condition

1 mL methanol/1 mL water

Load

1 mL spiked plasma

Wash

300 µL water

Elute

500 µL 1% glacial acetic acid

with 10% methanol

Evaporate and Reconstitute

Dilute and add internal standard:

480 µL mobile phase and

20 µL internal standard

0.015AU

Minutes

0 5 15

1

2

B

A

1. Acyclovir


Albuterol (Salbutamol)

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: Water/methanol/glacial acetic acid 69:30:1 with 5 mM sodium 1-hexanesulfonateFlow rate: 1.0 mL/minInjection volume: 10 µL of 200 µg/mL salbutamolDetection: UV @ 276 nm

USP Tailing Factors

1. 1.2

1. Salbutamol

Minutes

1

0 2 4 6 8

HN

CH3

CH3

HO

HO

HO


Albuterol (Salbutamol) in Serum

A

B

2015105

12

Minutes

0

100 mV




Salbutamol 0.400 98.8% 3.4%2.00 98.0% 3.5%

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ guard column, 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046980, Guard - WAT054250Mobile phase: 5 mM hexanesulfonate and 1% glacial acetic acid in

water/1% glacial acetic acid in methanol, 75:25Flow rate: 1.0 mL/minInjection volume: 20 µL of reconstituted porcine serum extractDetection: Fluorescence, Ex = 275 nm, Em = 310 nm

Compounds:1: Salbutamol2: Bamethan (I.S.)

Condition:1 mL methanol/1 mL water

Load:1 mL spiked porcine serum

with 1.0 µg/mL bamethan (I.S.)

Wash:1 mL 5% methanol in water

Elute:1 mL methanol

Evaporate and Reconstitute:

40 ˚C under nitrogen stream200 µL mobile phase

1. Salbutamol


2. Bamethan (I.S.)

HN

CH3

CH3

HO

HO

HO

Minutes


Alkaloids in Goldenseal

Oasis® HLB method for alkaloids in GoldensealConditions for Oasis® HLB cartridge, 3 cc, 60 mg


Condition/Equilibrate:

1 mL methanol/1 mL 150 mM K2HPO4

Load:

3 mL of diluted sample

Wash:

1 mL 30% methanol/ 150 mM K2HPO4

Elute:

3 mL methanol

0 5 10

Sample pre-preparation100 mg sample is extracted with 25 mL of ethanol:water (70:30)1 mL of the ethanolic extract is diluted 1:3 with water (~ pH 7)

• Recovery, measured with certified standards at 100 ppm in reagent water,was greater than 85 % for all compounds

• All analyses gave results within ± 35 % of the expected values with theexception of the liquid supplement (see goldenseal analysis)

• The selective SPE extraction and cleanup procedure provided a convenientanalysis of echinacea phenolics in complex matrix such as in herbal tea

HPLC Method

Column: Symmetry® C18, 4.6 x 250 mm, 5 µmPart number: WAT054275Mobile Phase A: 0.1% phosphoric acidMobile Phase B: AcetonitrileGradient: Time Profile

(min) %A %B0 90 1013 78 2240 60 40

Flow Rate: 1.5 mL/minInjection volume: 10 µLTemperature: 35° CDetection: UV @ 330 nm

Herbal tea extractbefore SPE cleanup

Herbal tea extract after SPE cleanupusing Oasis® MAX

Minutes

hydrastineberberine


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 20 mM potassium phosphate pH 7.0/ methanol 35:65Flow rate: 1.0 mL/minInjection volume: 10 µL of 100 µg/mL amoxapine and 100 µg/mL trazodoneDetection: UV @ 254 nm

USP Tailing Factors

1. 1.12. 1.4

1. Trazodone

2. Amoxapine

Amoxapine and Trazodone

Minutes


Amoxicillin

HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 10 mM sodium acetate, pH 4.0/acetonitrile 96:4Flow rate: 1.0 mL/minInjection volume: 10 µL of 100 µg/mL sampleDetection: UV @ 230 nm

USP Tailing Factors

1. 1.15

1. Amoxicillin

Minutes


HPLC Method

Column: Symmetry® C8 ,3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: 56 mM sodium phosphate, pH 4.4/methanol 95:5Flow rate: 1.0 mL/minInjection volume: 10 µL of 100 µg/mL amoxicillin and 25 µg/mL clavulante extracted tablet sample at 10 to 39 µg/mLDetection: UV @ 220 nm

USP Tailing Factors

1. 1.22. 1.1

1. Clavulanate

2. Amoxicillin

Amoxicillin and Clavulanate Potassium Augmentin Tablet

Minutes


Amoxicillinin in an Oral Suspension Formulation

HPLC Method


USP Tailing Factors

1. 1.13

1. Amoxicillin

Minutes


Ampicillin

HPLC Method


USP Tailing Factors

1. 1.07

1. Ampicillin

Minutes


Amphetamines

HPLC Method

Column: SymmetryShield™ RP18, 3.9 x 150 mm, 5 µm, Part Number: 186000108Mobile phase: 0.1% TFA in Water/acetontrile/methanol 91:7:2Flow rate: 1.0 mL/minInjection volume: 50 µLDetection: UV @ 210

USP Tailing Factors

1. 1.282. 1.323. 1.30

1. Ephedrine (I.S.)

2. Amphetamine

3. Methamphetamine

Minutes


Amphetamines in Human Urine

HPLC Method

Column: SymmetryShield™ RP18, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ Guard Column, 3.9 x 20 mm, 5 µmPart Numbers: Column - 186000108, Guard - 186000107Mobile phase: 0.1% TFA in Water/Acetontrile 90:10Flow rate: 1.0 mL/minInjection volume: 50 µL Temperature: 30˚ CDetection: UV @ 214 nm (0.14 AUFS)

Compounds:1. Ephedrine2. Amphetamine3. Methamphetamine

%Recovery (%RSD) Spike Levels: 0.7 µg/mL 3.5 µg/mL

Amphetamine (n=8) 99.3 (4.9) 104.7 (1.8)

Methamphetamine (n=8) 105.5 (5.8) 100.9 (4.4)

Amphetamine Interday (n=16) 102.8 (2.7)

Amphetamine Interperson (n=16) 98.8 (6.2) 101.8 (3.3)

Methamphetamine Interday (n=16) 98.5 (5.4)

Methamphetamine Interperson (n=16) 96.4 (11.5) 99.4 (6.3)

Ephedrine (I.S.) (n=8) 89.5 (1.4)

2 4 6 8

Minutes

0.14

AU

FS

12

3

B

A

Chromatogram of A) Spiked Urine, B) Blank Urine

1. Ephedrine (I.S.)

Oasis® HLB Extraction MethodOasis® HLB Extraction Plate, 30 mg/96-well


Conditioning:1 mL methanol

1 mL water

Load:2 mL of acidfied spiked human urine

Wash 1:1 mL 5% methanol with

2% ammonium hydroxide

2. Amphetamine 3. Methamphetamine

Wash 2:1 mL 20% methanol with 2% ammonium hydroxide

Elute:0.5 mL 20% methanol with

2% acetic acid

Minutes


Anticonvulsants

HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µmPart number: WAT046970Mobile phase: 100 mM potassium phosphate, pH 6.9/acetonitrile/water 20:30:50Flow rate: 1.0 mL/minInjection volume: 10 µL of11-160 µg/mL sampleTemperature: 30˚ CDetection: UV @ 214 nm

USP Tailing Factors

1. 1.412. 1.033. 1.114. 1.025. 1.07

1. Succinimide

2. Primidone

3. Phenobarbital

4. Mephenytoin

5. Mephobarbital

Minutes


HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µmPart number: WAT200655Mobile phase: 100 mM phosphate pH 7.0/acetonitrile/methanol 55:35:10Flow rate: 1.0 mL/minInjection volume: 100 µL acidified plasma sample solutionTemperature: 30˚ CDetection: UV @ 230 nm

Compounds:1. Nordoxepin2. Nortriptyline3. Norverapamil4. Doxepin5. Amitriptyline6. Verapamil7. Methoxyverapamil (I.S.)

Antidepressants in Plasma

Compound Concentration % Recovery %RSD

µg/mL (n=6)

Amitriptyline 1.46 99.9% 1.10%0.29 94.9% 0.60%

Doxepin 1.00 98.4% 0.69%0.20 98.0% 2.30%

Nordoxepin 0.50 92.8% 0.91%0.10 88.0% 1.33%

Nortriptyline 0.62 95.3% 1.29%0.12 91.1% 1.03%

Verapamil 2.50 96.7% 0.63%0.50 98.8% 0.70%

Norverapamil 1.00 95.9% 0.59%0.20 98.5% 1.04%


B.

A.

0 5 10 15Minutes

0.002 AU

1

6. Verapamil

3. Norverapamil




Load:1 mL of acidified plasma

sample solution

Wash:1 mL of 70% methanol,


Elute:0.5 mL of 70% methanol,

2% acetic acid

Evaporate and Reconstitute:Not required

7. Methoxyverapamil (I.S.)

1. Nordoxepin 2. Nortriptyline

5. Amitriptyline

2 34 5

6

7

4. Doxepin


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250 Mobile phase: 100 mM potassium phosphate, pH 6.9/acetonitrile/methanol/water 17:25:5:53Flow rate: 1.0 mL/minInjection volume: 5 µL of 25µg/mL sampleDetection: UV @ 214 nm

USP Tailing Factors

1. NA 5. 1.102. NA 6. 1.173. 1.13 7. NA4. 1.17 8. NA 1. 2-Phenyl-2ethylmalonamide

2. p-Hydroxyphenobarbital

3. Primidone

4. Phenobarbital

5. Carbamezapine-10,11-epoxide

6. Carbamezapine

Antiepileptics and Metabolites

Minutes

7. 10,11-Dihydrocarbamezapine 8. Phenytoin


Antipyrine and Its Metabolite

HPLC Method

Column: SymmetryShield™ RP8, 4.6 x 50 mm, 5µmPart Number: 186000224Mobile phase: 0.1% glacial acetic acid/methanol 85:15Flow rate: 1.0 mL/minInjection volume: 5 µL solution with antipyrine (240 ng) and 4-hydroxyantipyrine (29 ng)Detection: UV @ 254 nm

1. Antipyrine

2. 4-Hydroxyantipyrine

1

2

2 4

Minutes


Atrazine and Metabolites in Drinking Water

1

23

4 5

6

7

0 2010

Minutes

PDA

(0.

08 A

UFS

)

Spiked Sample

Blank Sample

Oasis® MCX SPE MethodConditions for Oasis® MCX Cartridge, 6 cc, 150 mg

Part Number 186000256

Compounds (% Recovery - % RSD, n=5)0.2 µg/L 1.0 µg/L

1. Hydroxydesisopropylatrazine 94 (3) 85 (3)2. Desethyldesisopropylatrazine 75 (8) 76 (5)3. Hydroxydesethylatrazine 89 (6) 76 (7)4. Desisopropylatrazine 79 (4) 83 (2)5. Hydroxyatrazine 107 (7) 101 (2)6. Desethylatrazine 79 (5) 83 (3)7. Atrazine 89 (5) 77 (3)

HPLC Method

Column: SymmetryShield™ RP18, 3.9 x 150 mm, 5 µmPart number: 186000108Mobile Phase A: 20 mM Phosphate buffer, pH 6.8Mobile Phase B: AcetonitrileGradient: Time Profile

(min) %A %B0 95 52 95 520 25 75

Flow Rate: 0.8 mL/minInjection volume: 80 µLDetection: PDA (215 nm)

Prepare Sample:adjust to pH 1.5 with HCI

Condition: 2 mL methanolRinse with 2 mL H2O

Load Sample

Wash #1:2 mL 0.1 N HCI

Wash #2:2 mL methanol

Elute:3 mL methanol (4% NH4OH)


Drinking water samples (100 mL) were spikedwith the herbicides and adjusted to pH 1.5. Thesamples were then analyzed using 6 ccOasis® MCX cartridges using the protocol forbasic compounds

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 100 mM Potassium phosphate, pH 6.9/acetonitrile/water 20:30:50Flow rate: 1.0 mL/minInjection volume: 10 µL of 25µg/mL sampleDetection: UV @ 214 nm

USP Tailing Factors1. 1.17 5. 1.112. 1.12 6. 1.113. 1.14 7. 1.094. 1.10 8. 1.09

1. Barbital 2. Allobarbital

3. Phenobarbital 4. Butabarbital

5. Butalbital 6. Amobarbital

Barbiturates

8. Secobarbital7. Mephobarbital


Barbiturates in Human Urine

%Recovery (n=8) (%RSD) (n=8)Compound 0.2 µg/mL 1.0 µg/mL

1. Phenobarbital 114.3 (1.7) 106.5 (0.5)

2. Butabarbital 95.7 (1.3) 105.5 (0.7)

3. Butalbital 109.5 (0.9) 104.2 (0.9)

4. Amobarbital (I.S.) 86.3 (1.7)

5. Mephobarbital 92.5 (3.6) 92.4 (1.7)

6. Secobarbital 101.5 (5.2) 94.8 (2.2)

1. Phenobarbital

HN

NH

OO

O

H3C

H C3

H3C

4. Amobarbital (I.S.)2. Butabarbital

HPLC Method

Column: SymmetryShield™ RP18, 2.1 x 150 mm, 5 µmGuard Column: Sentry™ Guard Column RP18, 3.9 x 20 mm, 5 µmPart numbers: Column - 186000111, Guard - 186000107Mobile phase: 50 mM potassium phosphate, pH 7.0/acetonitrile 71: 29Flow rate: 1 mL/minInjection volume: 80 µL urine extractTemperature: 30 ˚CDetection: UV @ 214 nm (0.350 AUFS)



Condition:1 mL of methanol

Equilibrate:1 mL water

Wash 1:1 mL of 5% methanol

Wash 2:1 mL 25% methanol with 2% acetic acid

Elute:1 mL 35% methanol with 2% ammonium hydroxide

Evaporated:To dryness under N2 at 40˚C

Load:2 mL water of spiked human urine

Reconstituted:300 µL of water

5. Mephobarbital3. Butalbital6. Secobarbital

0 8

BA

16

1

23

45

6

0.35

0 A

UFS

Minutes

Chromatogram of A) Blank Urine, B) Spiked Urine

Minutes


Beclomethasone

HPLC Method

Column: Symmetry® C18, 4.6 x 100 mm, 3.5 µmPart number: WAT066220Mobile phase: Acetonitrile/water 65:35Flow rate: 1.4 mL/minInjection volume: 15 µL of 0.1 mg/mL of each beclomethasone-dipropionate and testosterone propionate (internal standard)Detection: UV @ 254 nm

USP Tailing Factors1. 1.12. 1.0

1. Beclomethasone Dipropionate

2. Testosterone Propionate (I.S.)

Minutes

0 105

1

2


Benomyl and Bisphenol A

1

234

Minutes

0 5 10

sample

blank

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile Phase A: 10 mM phosphate, pH 6.8Mobile Phase B: MethanolGradient: Time Profile

(min) %A %B0 60 4020 0 100

Flow Rate: 1.0 mL/minInjection volume: 100 µLDetection: PDA (283 nm extracted)

Compounds % RECOVERY ± % RSD1. Benomyl 65 ± 102. Carbaryl N/A3. Atrazine N/A4. Bisphenol A 83 ± 2

100 ppb spike level in pear

Oasis® SPE Method for Endocrine DisruptorsConditions for Oasis® HLB Cartridge, 6 cc, 200 mg


Prepare Sample:adjust to pH 3

Condition:3 mL MTBE*


Load:up to 500 mL sample

Wash:3 mL 5% methanol in H2O

Elute:6 mL 10% methanol/MTBEt*


For GC analysis, dryextract over Na2SO4,

then adjust to 1 mL

For LC analysis, exchangeto acetonitrile, then

adjust to 1 mL

1. Benomyl 2. Carbaryl

3. Atrazine 4. Bisphenol A

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 mm x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: Water/acetonitrile/phosphoric acid 63:37:0.1Flow rate: 1.0 mL/minInjection volume: 10 µL of 50 µg/mL sampleDetection: UV @ 254 nm


2. Propylparaben(internal standard)

Betamethasone

1. Betamethasone

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: Water/acetonitrile/phosphoric acid 63:37:0:1Flow rate: 1.0 mL/minInjection volume: 10 µL of 150 µg/mL sampleDetection: UV @ 254 nm


1. Betamethasone

2. Propylparaben (I.S.)

Betamethasone in Syrup Formulation

Minutes

Celestone is a registered trademark of Schering Corporation.


HPLC Method

Column: Symmetry300™ C18, 4.6 x 50 mm, 5 µm Part number: WAT106209Mobile phase A: 0.1% TFA in waterMobile phase B: 0.1% TFA in acetonitrileGradient: Time Profile

(min) %A %B0 100 045 70 30

Flow rate: 1.0 mL/minInjection volume: 20 µLDetection: UV @ 214 nm

BSA Tryptic Digest

0.00 20.00 40.00

Minutes


HPLC Method

Column A: Symmetry300™ C18, 4.6 x 50 mm, 5 µm Column B: Symmetry300™ C18, 4.6 x 150 mm, 5 µmColumn C: Symmetry300™ C18, 4.6 x 250 mm, 5 µmPart numbers: A: WAT106209

B: WAT106157C: WAT106151

Mobile phase A: 0.1% TFA in waterMobile phase B: 0.1% TFA in acetonitrileGradient: Time Profile

(min) %A %B0 100 045 70 30

Flow rate: 0.75 mL/minInjection volume: 20 µL (7 µL for 4.6 x 50 mm)Temperature: 35˚CDetection: UV @ 214 nm

BSA Tryptic Digest - Column Length Effects

0.00 20.00 40.00

Minutes

0.00 20.00 40.00

Minutes

0.00 20.00 40.00

Minutes

A

B

C


HPLC Method


(min) %A %B0 100 045 70 30

Injection volume: 20 µLTemperature: 35˚CDetection: UV @ 214 nm

BSA Tryptic Digest - Flow Rate Effects

0.00 20.00 40.00

Minutes

0.00 20.00 40.00

Minutes

0.00 20.00 40.00

Minutes

0.00 20.00 40.00

Minutes

0.3 mL/min

0.5 mL/min

1.0 mL/min

2.0 mL/min


HPLC Method


(min) %A %B0 100 045 70 30

Flow rate: 0.75 mL/minInjection volume: 20 µLTemperature: 35˚CDetection: UV @ 214 nm

BSA Tryptic Digest - Gradient Duration Effects

0.00 20.00 40.00

Minutes

0.00 20.00 40.00

Minutes

0.00 20.00 40.00

Minutes

0.00 20.00 40.00

Minutes

0.00 20.00 40.00

Minutes

Gradient time: 15 min.






Bupropion

HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 20 mM potassium phosphate, pH 7.0/methanol 35:65Flow rate: 1.0 mL/minInjection volume: 10 µL of 20 µg/mL sampleDetection: UV @ 254 nm

USP Tailing Factors1. 105

1. Bupropion

Minutes


Busiperone

HPLC Method

Column: SymmetryShield™ RP18, 4.6 x 150 mm, 5 µm Part number: 186000109Mobile phase: 20 mM phosphate buffer, pH 7.0/acetonitrile 55:45Flow rate: 1.0 mL/minInjection volume: 5 µLDetection: UV @ 240 nm

USP Tailing Factors1. 1.08

1. Busiperone

Minutes


Caffeine and Metabolites in Serum




Theobromine 0.100 103.0% 3.4%0.500 104.0% 2.4%

Paraxanthine 0.100 101.0% 6.2%0.500 98.9% 2.3%

Theophylline 0.100 100.0% 5.2%0.500 101.0% 2.1%

Caffeine 0.100 92.6% 4.4%0.500 97.5% 3.2%

HPLC Method

Column: SymmetryShield™ RP8, 3.0 x 150 mm, 5 µmGuard Column: Sentry™ guard column, 3.9 x 20 mm, 5 µmPart numbers: Column - WAT094243, Guard - WAT200675Mobile phase: 20 mM ammonium acetate, pH 5/acetonitrile, 95:5Flow rate: 0.6 mL/minInjection volume: 20 µL of reconstituted porcine serum extract Temperature: 25˚ CDetection: UV @ 273 nm

Compounds:1: Theobromine2: Paraxanthine3: Theophylline4: β-hydroxyethyltheophylline (I.S.)5: Caffeine


Load1 mL porcine serum with 0.2 µgß-hydroxyethyltheophylline (I.S.)

Wash1 mL water

Elute1 mL methanol


200 µL mobile phase

1. Theobromine


3. Theophylline2. Paraxanthine

4. ß-hydroxyethyltheophylline (I.S.)

N

NN

N

O

O CH2CH2OH

H3C

CH3

5. Caffeine

N

NN

N

O

O CH2

H3C

CH3

B

A

0.03 AU

0 5 10 15

1

2

3

4

5

Minutes


Captopril

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: 0.1% phosphoric acid in water/methanol 60:40Flow rate: 1.0 mL/minInjection volume: 10 µL of 200 µg/mL captopril and 20 µg/mL of captopril disulfideTemperature: 40˚ CDetection: UV @ 220 nm

USP Tailing Factors:1. 1.02. 1.2

1. Captopril

Minutes


Carbadox

HPLC Method

Column: Symmetry® C18, 4.6 x 100 mm, 3.5 µmPart number: WAT066220Mobile phase: 20 mM ammonuim acetate, pH 5.0/Acetonitrile 85:15Flow rate: 1.4 mL/minInjection volume: 15 µL of 0.025 mg/mLTemperature: 30˚ CDetection: UV @ 254 nm


1. Carbadox

Minutes


Catechins - 4.6 x 20 mm Intelligent Speed™ Separation

HPLC Method

Columns: Symmetry® C18, 4.6 x 20 mm, 3.5 µm IS™

SymmetryShield™ RP18, 4.6 x 20 mm, 3.5 µm IS™

Part numbers: Symmetry - 186002090, Shield - 186002092Mobile phase A: 0.1% HCOOH in WaterMobile phase B: 0.1% HCOOH in MeOHGradient: Time Profile

(min) %A %B0.0 100 04.0 60 40


Compounds:1. Caffeine2. Epicatechin3. Epigallocatechin Gallate

Minutes

t0= 0.13 minMax psi= 2225

1

2 3

0.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.000.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00

3

1

2

0.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.000.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00

Minutes

t0= 0.13 minMax psi= 2111

SymmetryShield™ RP18

Symmetry® C18

OOH

OH

O

OH

OH

OH

OOH

OH

OH

OOH

OH

OH

OH

OH

N

NN

N

O

O CH2

H3C

CH3

3. Epigallocatechin Gallate2. Epicatechin1. Caffeine


Cefixime

HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 10 mM sodium acetate, pH 3.8/acetonitrile 80:20Flow rate: 1.0 mL/minInjection volume: 10 µL of 100 µg/mL extracted suspension sampleDetection: UV @ 254 nm


1. Cefixime

Minutes


Cefuroxime

HPLC Method



1. Cefuroxime

Minutes


Cephalexin

HPLC Method

Column: Symmetry® C18, 3.0 x 150 mm, 5µmPart number: WAT054200Mobile phase: 1.25% glacial acetic acid in water/methanol 88:12Flow rate: 0.6 mL/minInjection volume: 400 µL of cephalexin (1 mg/mL) and 200 µL of 1-hydroxybenzotriazole (Internal standard, 1 mg/mL)Detection: UV @ 254 nm


1. 1-hydroxybenzotriazole (IS)

2. Cephalexin

1

100

2

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150mm, 5 µmGuard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: Water/methanol/glacial acetic acid 55:45:0.1Flow rate: 1 mL/minInjection volume: 10 µL of 100 µg/mLDetection: UV @ 280 nm


1. Chloramphenicol

Chloramphenicol

Minutes


Chlordiazepoxide and Metabolites

HPLC Method

Column: Symmetry® C18, 3.0 x 150 mm, 5 µmPart number: WAT054200Mobile phase: 20 mM Potassium phosphate pH 7.0/methanol/acetonitrile 49:28:23Flow rate: 0.59 mL/minInjection volume: 5 µL of 40 74 µg/mLDetection: UV @ 240 nm

USP Tailing Factors1. 1.12. 1.23. 1.14. 1.25. 1.1

1. Norchlordiazepoxide

2. Oxazepam

3. Noradiazepam

4. Chlordiazepoxide

5. Demoxepam

impurity

5 10

1

2

3

45

Minutes


Chlordiazepoxide and Metabolites in Serum




1. Norchlordiazepoxide 0.200 97.8% 4.3%0.040 96.5% 5.5%

2. Oxazepam 0.200 104.0% 2.6%0.040 90.0% 2.5%

3. Nordazepam 0.200 101.0% 3.0%0.040 98.9% 1.2%

4. Chlordiazepoxide 0.200 90.0% 2.4%0.040 100.0% 4.1%

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ guard column, 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046980, Guard - WAT054225Mobile phase: 20 mM Potassium phosphate, pH 7.0/acetonitrile/methanol 56:21:23Flow rate: 1.0 mL/minInjection volume: 20 µL of reconstituted porcine serum extractDetection: UV @ 240 nm

Compounds:1: Norchlordiazepoxide2: Oxazepam3: Nordazepam4: Chlordiazepoxide5: Demoxepam (I.S.)


Load:1 mL spiked porcine serum

with 1.5 µg/mL demoxepam (I.S.)

Wash:1 mL 5% methanol in water

Elute:1 mL methanol

Evaporate and Reconstitute:40 ˚C under nitrogen stream

200 µL of 20 mM potassium phosphate pH7/methanol 80:20 (v/v)

5. Demoxepam


4. Chlordiazepoxide3. Nordazepam1. Norchlordiazepoxide 2. Oxazepam

N

N

Cl

OH

2 3

4

1

5

5 10 15 20

0.002 AU

Minutes

B

A

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µmPart number: WAT046970Mobile phase: 50 mM potassium phosphate, pH 3.0/ acetonitrile 80:20Flow rate: 1.0 mL/minInjection volume: 5 µL of 120 µg/mL sampleDetection: UV @ 261 nm


1. Chlorpheniramine Maleate

Chlorpheniramine

Minutes


Cimetidine- (SymmetryShield™ RP18)

HPLC Method

Column: SymmetryShield™ RP18, 4.6 x 250 mm, 5 µmPart number: 18600012Mobile phase: 0.3 mL phosphoric acid, methanol/water 18:82Flow rate: 1.8 mL/minInjection volume: 50 µL Detection: UV @ 220 nm


1. Cimetidine

0 1 2 3Minutes


Cimetidine - Ion-Pair Separation

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: 6.6 mM sodium 1-hexanesulfanate, 0.04% phosphoric acid in water/methanol 76:24Flow rate: 1.0 mL/minInjection volume: 10 µL of 100 µg/mLDetection: UV @ 220 nm


1. Cimetidine

Minutes


Cimetidine- (Symmetry® C18 )

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: 0.03% Phosphoric acid in water/methanol 90:10Flow rate: 1.0 mL/minInjection volume: 10 µL injection of 10 µg/mLDetection: UV @ 220 nm


1. Cimetidine

1

1 432

Minutes


Clobetasol and Related Compound

HPLC Method

Column: SymmetryShield™ RP18, 4.6 x 150 mm, 5 µmPart number: 186000109Mobile phase: Acetonitrile/water/methanol 48:42:10Flow rate: 1.0 mL/minInjection volume: 10 µLDetection: UV @ 240 nm


1. Clobetasol

2. Beclomethasone

Minutes


Clonazepam

HPLC Method

Column: Symmetry® C18, 4.6 x 250 mm, 5 µmPart number: WAT054275Mobile phase: Water/methanol/acetonitrile 40:30:30Flow rate: 1.5 mL/minInjection volume: 25 µL of sample with 40 µg/mL of clonazepam and 80 µL/mL of o-dichlorobenzene (internal standard)Detection: UV @ 254 nm


1. Clonazepam

2. O-dichlorobenzene (IS)

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046980, Guard - WAT054225Mobile phase: 20 mM potassium phosphate, pH 2.18/methanol 75:25Flow rate: 1.0 mL/minInjection volume: 5 µL of 200 µg/mL sampleDetection: UV @ 254 nm


Cocaine

N

O

Me

OMeO

O1. Cocaine

Minutes


Cocaine and its Metabolites in Serum




1. Benzoylecgonine 2.00 93.7% 1.7%0.40 93.6% 2.2%

2. Cocaine 2.00 98.0% 1.1%0.40 93.4% 2.9%

3. Cocaethylene 2.50 97.7% 2.8%0.50 98.2% 5.1%

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ guard column, 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250 Mobile phase A: 20 mM potassium phosphate, pH 7 Mobile phase B: MethanolGradient: Time Profile

(min) %A %B0 78 228.5 78 228.6 42 5830 42 58

Flow rate: 1.0 mL/minInjection volume: 1 mL of reconstituted porcine serum extract Detection: UV @ 235 nm


Load1 mL serum spiked porcine sample

with 20 µL phosphoric acid


Elute1 mL methanol


40 ˚C under nitrogen stream250 µL water:methanol 80:20 (v/v)

1. Benzoylecgonine


N

O

Me

OMeO

O

2. Cocaine 3. Cocaethylene

N

O

Me

OO

O

2

3

1

AB

5

0.01. AU

20 251510MinutesMinutes


Codeine and Its Glucuronide Metabolite in Human Urine

Compound % Recovery %RSD 0.12 µg/mL 0.6 µg/mL

Codeine (n=3) 88.5 (2.7) 99.5 (1.2)

Codeine-6-Glucuronide (n=3) 99.3 (5.4) 98.7 (0.4)

Codeine Interday (n=6) 102.5 (3.5) 105.4 (4.0)

Codeine Interperson (n=9) 91.6 (7.1) 104.1 (5.4)

C-6-G Interday (n=6) 116.1 (9.4) 111.5 (3.3)

C-6-G Interperson (n=9) 102.4 (7.7) 107.4 (7.3)

HPLC Method

Column: Symmetry® C18, 2.1 x 150 mm, 3.5 µmGuard Column: Symmetry® C18, 2.1 x 10 mm, 3.5 µmPart numbers: Column - 186000174, Guard - 186000169Mobile phase: Methanol/Acetonitrile/0.05% TFA in water 5:5:90Flow rate: 0.3 mL/minInjection volume: 80 µL urine extractTemperature: 30˚ CDetection: UV @ 220 nm (0.04 AUFS)

Compounds:1. Ranitidine (I.S.)2. Codeine-6-Glucuronide (C-6-G)3. Codeine

Chromatogram of Urine Extracts: A) Blank B) Spiked Sample

CH3O

O H

NCH3

HO

3. Codeine2. Codeine-6-Glucuronide(C-6-G)

O

OH OH

OH

OHOC

O

O

H3CO

N-

H

CH3

Oasis® MCX Extraction MethodOasis® MCX Extraction Cartridge, 3 cc/60 mg


Load3 mL acidified spiked human urine

Wash 12 mL 0.1N hydrochloric acid

Wash 22 mL methanol

Elute2 mL 5% ammonium hydroxide

with 95% methanol

After elution, the extract is diluted 1:3 with water for HPLC analysis

No Conditioning

Minutes0 105

1

2

3

nonspiked sample

spiked sample0.04

AU

FS

1. Ranitidine

Minutes


Codeine and Its Glucuronide Metabolite in Porcine Plasma

HPLC Method

Column: Symmetry® C18, 2.1 x 150 mm, 3.5 µmGuard Column: Symmetry® C18, 2.1 x 10 mm, 3.5 µmPart numbers: Column - 186000174, Guard - 186000169Mobile phase: Methanol/Acetonitrile/0.05% TFA in water 5:5:90Flow rate: 0.3 mL/minInjection volume: 80 µL urine extractTemperature: 30˚ CDetection: UV @ 220 nm (0.04 AUFS)

Compounds:1. Ranitidine (I.S.)2. Codeine-6-Glucuronide (C-6-G)3. Codeine




No Conditioning

Wash 1

2 mL 0.1N hydrochloric acid

Wash 2

2 mL methanol

Elute

2 mL 5% ammonium hydroxide

with 95% methanol

After elution, the extract is diluted 1:3 with water for HPLC analysis

Load

3 mL acidified plasma sample

CH3O

O H

NCH3

HO

3. Codeine2. Codeine-6-Glucuronide(C-6-G)

O

OH OH

OH

OHOC

O

O

H3CO

N-

H

CH3

1. Ranitidine

% Recovery(n=3) %RSD(n=3) Spike Level: 0.12 µg/mL 0.6 µg/mL

Codeine 95.4 (5.0) 103.4 (0.9)

Codeine-6-Glucuronide 106.8 (1.9)1 04.6 (1.3)

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 7.4 mM sodium 1-heptanesulfonate in water/acetonitrile 65:35Flow rate: 1.0 mL/minInjection volume: 8 µL of 100 µg/mL sampleDetection: UV @ 230 nm


2. Chlorcyclizine HCL

Cyclizine and Chlorcyclizine

1. Cyclizine

Minutes


Cytochrome c Tryptic Digest - Column Lifetime Study, Critical Pair Resolution

HPLC Method

Column: Symmetry300™ C18, 3.9 x 150 mm, 5 µmPart number: WAT106154Mobile phase A: 0.1% TFA water/acetonitrile 90:10Mobile phase B: 0.1% TFA water/acetonitrile 40:60Gradient: Time Profile

(min) %A %B0 100 045 34 66


Minutes Minutes


Cytochrome c Tryptic Digest - Pore Size Effects

HPLC Method

Column: Symmetry® C18, 4.6 x 150 mm, 5 µm, 100ÅGuard Column: Symmetry300™ C18, 4.6 x 150 mm, 5 µm, 300ÅPart numbers: Column - WAT045905, Guard - WAT106157Mobile phase A: 0.1% TFA in WaterMobile phase B: 0.1% TFA in AcetonitrileGradient: Time Profile

(min) %A %B0 100 050 70 30


Symmetry® C18, 4.6 x 150 mm, 5 µm, 100Å

0.00 20.00 40.00

Minutes

0.00 20.00 40.00

Minutes

Symmetry300™ C18, 4.6 x 150 mm, 5 µm, 300Å


Cytochrome c Tryptic Digest -Recovery Study

HPLC Method

Column: Symmetry300™ C18, 4.6 x 50 mm, 5 µmPart number: WAT106209Mobile phase A: 0.1% TFA in WaterMobile phase B: 0.1% TFA in AcetonitrileGradient: Time Profile

(min) %A %B0 100 045 70 30


FirstRun

SecondRun

TFA Blank InjectionMinutes


Cytochrome c Tryptic Digest - Reproducibility Study

HPLC Method

Column: Symmetry300™ C18, 3.9 x 150 mm, 5 µmPart number: WAT106154Mobile phase A: 0.05% TFA in WaterMobile phase B: 0.1% TFA in AcetonitrileGradient: Time Profile

(min) %A %B0 100 045 72 28


Batch 107

Batch 106

Batch 104

Batch 103

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 23 mM ammonium nitrate, pH 3.4/acetonitrile 30:70Flow rate: 1.0 mL/minInjection volume: 20 µL of 100 µg/mL sampleDetection: UV @ 254 nm


1. Dextromethorphan

Dextromethorphan

1

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 23 mM ammonium nitrate, pH 3.4/acetonitrile 30:70Flow rate: 1.0 mL/minInjection volume: 20 µL of 100 µg/mL sampleDetection: UV @ 254 nm


1. Dextromethorphan

Dextromethorphan in a Cough Syrup

Minutes


Diazepam in Serum - LC/MS

HPLC Method

Column: Symmetry® C18, 2.1 x 100 mm, 3.5 µmPart number: WAT058965Mobile phase: 2 mM Ammonium Acetate/Acetonitrile/Formic Acid 65:35:0.1Flow rate: 200 µL/minInjection volume: 10 µLMS: Micromass Quattro LCIon Mode: ES+Cone Voltage: 45 VCollision Energy: 25 eV

Diazepam

60 80 100 120 140 160 180 200 220 240 260 280 300 320 340m/z0

100

%

285.1

287.1

60 80 100 120 140 160 180 200 220 240 260 280 300 320 340m/z0

100

%

154.1

285.4

222.4193.4

182.0167.0

228.2 257.3

0.0 0.5 1.0 1.5 2.0 2.5 3.0

3.5

4.0 4.5 5.0ng/mL-0.399

771

Response

0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0ng/mL-0.399

165

Response

1.00 2.00 3.00 4.00Time0

100

%

2.26

1.00 2.00 3.00Time0

100

%

2.27

1.00 2.00 3.00 4.00Time0

100

%

2.2839

A B C

N

N

Cl

O3CH

Precursor(m/z)285

Product(m/z)154

Oasis® HLB Extraction MethodOasis® HLB 1 cc/30mg Extraction Cartridge



Wash: 1 mL 5% methanol in water

Elute:1 mL methanol

Load:1 mL porcine serum

Evaporate and Reconstitute:40˚ C under nitrogen stream,


Figure 1: Background-subtracted electrospray mass spectrum of pure diazepam standard (5µg), under optimum conditions. Chromatographed as described above to remove contaminants.

Figure 2: Background-subtracted electrospray product tion spectrum of pure diazepam standard (5µg), under optimum conditions. Chromatographed as described above to remove contaminants.

Figure 4: MRM Chromatograms under optimum conditions of pure diazepam standard at (A) 0.2ng/mL (LOD) and (B) 5.0ng/mL and (C) a processed human plasma sample with

a low concentration of diazepam (calculated as 0.75ng/mL)

Compound 3 name: DiazepamCoefficent of Determination: 0.998439Calibration curve: 150.210* x + -0.398957Response type: External Std., AreaCurve type: Linear, Origin: Exclude, Weighting: 1/x Axis trans: None

Figure 3: Calibration curve with triplicate injections for each point and demonstrating LOQ at 0.2ng/mL


Diclofenac Sodium

HPLC Method

Column: SymmetryShield™ RP18, 4.6 x 150 mm, 5 µmPart number: 186000109Mobile phase: 20 mM phosphate buffer, pH 7.0/acetonitrile 65:35Flow rate: 1.0 mL/minInjection volume: 5 µLDetection: UV @ 220 nm

USP Tailing Factor1. 1.18

1. Diclofenac

1

0 1 632 4 5

Minutes


Dihydroergotamine Mesylate

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: 50 mM ammonium phosphate, pH 5.8/Acetonitrile 35:65Flow rate: 1.0 mL/minInjection volume: 10 µL of 100 µg/mL dihydroergotamine mesylateDetection: UV @ 281 nm


1. Dihydroergotamine mesylate

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 100 mM sodium acetate, 5mM camphosulfonic acid, pH 6.2/acetonitrile/methanol 40:30:30Flow rate: 1.0 mL/minInjection volume: 10 µL of 50 µg/mL sampleDetection: UV @ 254 nm


1. Dilitiazem HCL

Diltiazem HCL

Minutes


Diltiazem HCL- Isolation of Impurities, Transfer fromAnalytical to Prep Columns

HPLC Method

Column: A. Symmetry® C18, 3.9 x 150 mm, 5 µmB. SymmetryPrep™ C18, 7.8 x 150 mm, 7 µmC. SymmetryPrep™ C18, 19 x 150 mm, 7 µm

Part numbers: A. WAT046980B. WAT066288C. WAT066240

Mobile phase: Acetonitrile/0.1% TFA in water 30:70Flow rates: A. 0.7 mL/min B. 2.8 mL/min C. 16.6 mL/minInjection volume: Diltiazem: A. 0.5 mg B. 2.0 mg C. 11.9 mgDetection: UV @ 280 nm

1. Diltiazem Hydrochloride

B. SymmetryPrep™ C18 ,7 µm, 7.8 mm x 150 mm

A. Symmetry® C18 ,5 µm, 3.9 mm x 150 mm

C. SymmetryPrep™ C18 ,7 µm, 19 mm x 150 mm

Minutes


Diphenoxylate HCL

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: 50 mM potassium phosphate, pH 6.0/acetonitrile 30:70Flow rate: 1.0 mL/minInjection volume: 10 µL of 100 µg/mL Diphenoxylate hydrochlorideDetection: UV @ 210 nm


1. Diphenoxylate HCL

Minutes


Disopyramide

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: 50 mM potassium phosphate, pH 7.0/methanol 70:30Flow rate: 1.0 mL/minInjection volume: 20 µL of 100 µg/mL sampleDetection: UV @ 254 nm


1. Disopyramide

Minutes


Doxepin in Serum




Doxepin 0.200 95.8% 1.4%4.00 96.6% 1.9%

HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ Guard Column, 3.9 x 20 mm, 5 µmPart numbers: Column - WAT200655, Guard - WAT200675Mobile phase: 20 mM potassium phosphate, pH 7/methanol 38:62Flow rate: 1.0 mL/minInjection volume: 20 µL of reconstituted porcine serum extractTemperature: 30˚ CDetection: UV @ 254 nm

Compounds:1: Butyl paraben (I.S.)2: Doxepin




Elute1 mL methanol with 5 µg

butyl paraben (I.S.)


200 µL methanol

2. Doxepin


1

0.001 AU

2

0 4 8 12Minutes

AB

1. Butyl paraben

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µmPart number: WAT046970Mobile phase: 10 mM potassium phosphate, pH 2/acetonitrile 75:25Flow rate: 2 mL/minInjection volume: 2 µL of 1.67 mg/mLTemperature: 80˚ CDetection: UV @ 215 nm

Compounds1. Maleic Acid2. Enalapril

Enalapril

2. Enalapril1. Maleic Acid

Minutes


Endocrine Disruptors in Soil

1

2

3

4

Minutes

0 5 10

sample

blank

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046970Mobile Phase A: 10 mM phosphate pH 6.8Mobile Phase B: MethanolGradient: Time Profile

(min) %A %B0 60 4020 0 100

Flow Rate: 1.0 mL/minInjection volume: 100 µLSample: 10 g potting soil extracted with 25 mL

acetonitrile; then SPE on Oasis® HLBDetection: PDA (225 nm extracted, 0.04 AUFS)

50 ppb spike levelCompounds % Recovery ± % RSD1. benomyl 62 ± 62. carbaryl 91 ± 43. atrazine 84 ± 54. bisphenol A 78 ± 6

Soil samples (5 g) were spiked with the appropriate compounds and extracted with 25 mL of acetonitrile (30 minutes on shaker). A 5 mL aliquotof the acetonitrile extract was diluted to 100 mL with reagent water (MilliQ)and then processed by SPE.

Oasis® SPE Method for Endocrine DisruptorsConditions for Oasis® HLB Cartridge, 6 cc, 200 mg


Prepare Sample:adjust to pH 3

Condition:3 mL MTBE*


Load:up to 500 mL sample

Wash:3 mL 5% methanol in H2O

Elute:6 mL 10% methanol/MTBEt*


For GC analysis, dryextract over Na2SO4,

then adjust to 1 mL

For LC analysis, exchangeto acetonitrile, then

adjust to 1 mL

1. Benomyl 2. Carbaryl 3. Atrazine 4. Bisphenol A

Minutes


Enkephalins

Peptides

1: Met enkephalin: Tyr-Gly-Phe-Met

2: Leu enkephalin: Tyr-Gly-Gly-Phe-Leu

HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase A: 0.1% TFAMobile phase B: 0.1% TFA in acetonitrile/water 90:10Gradient: Time Profile

(min) %A %B0 80 2030 40 60

Flow rate: 1.0 mL/minInjection volume: 5 µL of mixture with 500 µg/mL of each peptideDetection: UV @ 214 nm


Minutes


Etodolac

HPLC Method



1. Etodolac

Minutes


Flavonoids in Ginkgo

1

2

3

Minutes10 2010

HPLC Method

Column: Symmetry® C18, 4.6 x 250 mm, 5 µmPart number: WAT054275Mobile Phase: 0.5% Phosphoric acid/Methanol 50:50Flow Rate: 1.5 mL/minInjection volume: 10 µLTemperature: 25° CDetection: UV @ 270nm 0.02 AUFS

Sample pre-preparation1 g sample is refluxed in 50 mL of ethanol:3M HCl (70:30) for 2.5 hrThe cooled sample is adjusted to exactly 100 mL0.3 mL of the ethanolic extract is diluted 1:10 with water

• Recovery, measured with certified standards at 100 ppm in reagent water, was 82 % for quercitin

and > 90 % for the other compounds

• All analyses gave results within ± 40 % of the expected values with the exception of the

capsule (+ 60%)

• The selective SPE extraction and cleanup procedure provided a convenient analysis of ginkgo

flavonoids in a complex matrix (Herbal One with 16 herbal ingredients)

Oasis® HLB method for flavonoids in ginkgo

Conditions for Oasis® HLB cartridge, 3 cc, 60 mgPart Number WAT094226

Condition/Equilibrate:1 mL methanol/1 mL water

Load:3 mL of diluted sample

Wash 1:2 mL 5% methanol/water

Wash 2: 2 ml methanol/50mM NH4OAc (30:70) pH 5

Dry Cartridge:air dry for 15 min with vacuum

Elute:3 ml MTBE/methanol (80:20)

Evaporate and Reconstitute:1 mL mobile phase

Compounds % RECOVERY1. quercetin 82%2. kaempferol > 90%3. isorhamnetin > 90%total: 11 mg / tablet

1. Quercetin 2. Kaempferol

Minutes


Flunitrazepam

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: 50 mM potassium phosphate pH 6.0/acetonitrile 60:40Flow rate: 1.0 mL/minInjection volume: 10 µL of 30 µg/mL flunitrazepamDetection: UV @ 219 nm


1. Flunitrazepam

N

NO

FO2N

Minutes


Flunitrazepam and Related Compounds

Condition:

1 mL methanol

Equilibrate:

1 mL water

Load:

250 µL

Wash:

1 mL, 10% methanol with acetic acid

Elute 1 mL, 40% methanol with

ammonium hydroxide

Compound % Recovery

7-Amino Nitrazepam 118

7-Amino Clonazepam 100

7-Amino Flunitrazepam 95.9

Nitrazepam 93.7

Clonazepam 101

Flunitrazepam 85.9

Flunitrazepam

N

NO

FO2N

Minutes

1

1

2

2

3

3

4

4

5

5

6

6

7 8 9 10

HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µmPart number: WAT200655Mobile phase: Water/Acetonitrile 70:30Flow rate: 1.5 mL/minInjection volume: 100 µLTemperature: AmbientDetector: UV @ 220 nm

Compounds: 1. 7-Amino Nitrazepam2. 7-Amino Clonazepam3. 7-Amino Flunitrazepam4. Nitrazepam5. Clonazepam6. Flunitrazepam

Data supplied by J. Vukovik, L. SchofieldWaters Ltd., Canada

Oasis® HLB Extraction MethodOasis® HLB Extraction Plate,30 mg 96-well


Minutes


Four Drug Mixture-Warfarin, Dextromethorphan, Triprolidine, andTetracaineHPLC Method

Column: SymmetryShield™ RP18, 3.9 x 150 mm, 5 µmPart number: 186000108Mobile phase A: 25 mM Potassium phosphate, pH 7Mobile phase B: MethanolGradient: Time Profile

(min) %A %B0 85 1526 20 80

Flow rate: 1.0 mL/minInjection volume: 10 µL of mixture with 0.3 mg/mL triprolidine, 0.4 mg/mL dextromethorphan,

0.15 mg/mL tetracaine, and 0.05 mg/mL of warfarinDetection: UV @ 280 nm

USP Tailing Factors1. 1.32. 1.63. 1.14. 1.2

1. Warfarin

2. Dextromethorphan HCL

3. Triprolidine HCL

4. TetracaineMinutes


Furosemide

HPLC Method



1. Furosemide

Minutes


Hydrocortisone and Relate Compound

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: Acetonitrile/water 35:65Flow rate: 1.0 mL/minInjection volume: 10 µL of 10 µg/mL hydrocortisone and 30 µg/mL hydrocortisone-21-acetateDetection: UV @ 254 nm


2. Hydrocortisone-21-Acetate1. Hydrocortisone

Minutes


Ibuprofen and Naproxen in Serum




Naproxen 0.100 90.0% 4.0%0.500 98.7% 1.9%2.00 99.2% 0.85%

Ibuprofen 0.500 86.8% 4.6%2.50 95.0% 3.7%


Load

1 mL spiked porcine serum acidified with

20 µL of phosphoric acid

Wash

1 mL 5% methanol in water

Elute

1 mL methanol


40 ˚C under nitrogen stream

200 µL of mobile phase

1. Naproxen

O

OH

CH3

CH3

O

OH

CH3

CH3

2. Ibuprofen


0 5 10 15

Minutes

BA

HPLC Method

Column: SymmetryShield™ RP8, 3.0 x 150 mm, 5 µmGuard Column: Sentry™ Guard column, 3.9 x 20 mm, 5 µmPart Numbers: Column - WAT094243, Guard - WAT200675Mobile phase: 1.2% glacial acetic acid in water, Acetonitrile 50:50Flow rate: 0.6 mL/minInjection: 20 µL of reconstituted porcine serum extract Temperature: 25 ˚CDetection: UV @ 254 nm

Compounds:

1: Naproxen2: Ibuprofen


Insulin Chain - QC Batch Test for Symmetry300™ HPLC Columns

HPLC Method

Column: Symmetry300™ C4 , 3.9 x 150 mm, 5 µmPart number: WAT106154Mobile phases: A. 25% of 0.05% TFA in Acetonitrile / 75% of 0.05% TFA in Water

B. 32% of 0.05% TFA in Acetonitrile/ 68% of 0.05% TFA in Water (Linear Gradient from 100% A to 100% B in 14 Min.) Flow rate: 1.0 mL/minInjection volume: 4 µg, 10 µLDetection: UV @ 220 nm

Compounds:1. Insulin2. Desamino3. Deoxidized

Batch 3

Batch 2

Batch 1


Insulin- Impurity Isolation, Transfer from Analytical to Prep

HPLC Method

Columns: A. Symmetry® C18, 4.6 x 150 mm, 5 µmB. SymmetryPrep™ C18, 7.8 x 300 mm, 7 µmC. SymmetryPrep™ C18, 19 x 150 mm, 7 µm

Part numbers: A. WAT045905B. WAT066235C. WAT066240

Mobile phases: A. 0.1% TFA in Water B. 0.1% TFA/acetonitrile 26% B to 33% B in 14 minutes adjusted for gradient delay on prep system

Flow rates: A. 1.0 mL/min b. 5.76 mL/min c. 17mL/min Detection: UV @ 280 nmSample Load: Bovine pancreas insulin, 10 mg/mL

A. 0.07 mg b. 3 mg c. 8.5mgHPLC Systems: A. analytical system B. and C. prep system with 0.04 in. I.D. tubing

Compounds:

1. Insulin A and B chains with 51 residues, 5733 daltons2. Impurity

A. Symmetry® C18 , 5 µm, 4.6 mm x 150 mm

B. SymmetryPrep™ C18 , 7 µm, 7.8 mm x 300 mm

C. SymmetryPrep™ C18 , 7 µm, 19 mm x 150 mm

Minutes


Insulin- Isophase Suspension

HPLC Method

Column: Symmetry® C18, 4.6 x 150 mm, 5 µmPart number: WAT045905Mobile phase A: 0.1% TFA in Water Mobile phase B: Acetonitrile with 0.1% TFAGradient: Time Profile

(min) %A %B0 100 020 40 60

Flow rate: 1.0 mL/minInjection volume: 5 µL of sample with 150 µL of insulin suspension and 300 µL of 0.01N HCL

Suspension contains zinc-insulin crystals and protamine sulfate in buffered watersDetection: UV @ 280 nm

USP Tailing Factors1. 1.12. 1.23. 1.2

Compounds: 1. Unknown2. Insulin A and B chains with 51 residues,

5733 daltons3. Unknown

Minutes


Ketoconazole

HPLC Method

Column: SymmetryShield™ RP18, 4.6 x 250 mm, 5 µmPart number: 186000112Mobile phase: 70% diisopropylamine solution/30% ammonium acetate solution

Diisopropylamine solution: 2 mL diisopropylamine in 1 L methanolAmmonium acetate solution: 1 g in 200 mL of water



1. Ketoconazole

2. Terconazole

Minutes


Lidocaine HCL

HPLC Method

Column: SymmetryShield™ RP18, 4.6 x 250 mm, 5 µmPart number: 186000112Mobile phase: 50 mL glacial acetic acid in 930 mL of water, pH adjusted

to 3.4 with 0.1 N sodium hydroxide/70% buffer/30% acetonitrileFlow rate: 1.5 mL/minInjection volume: 20 µLDetection: UV @ 254 nm


1. Lidocaine HCL

2. Methylparaben

Minutes


Lifetime of Symmetry® 3.5 µm Column: 10,000Injections of Sulfa Drugs

HPLC Method

Column: Symmetry® 3.5µm C18, 4.6 x 100 mm Guard Column: Sentry™ Guard column, 3.9 x 20 mm, 5 µmPart numbers: Column - WAT066220, Guard - WAT054225Mobile phase: Water/methanol/glacial acetic acid 79:20:1Flow rate: 1.5 mL/minInjection volume: 10 µL of mixture of six sulfa drugs at 10 to 39 µg/mLDetection: UV @ 254 nm

SNH

O

O

N

N

NH2SNH

O

O

N

N

NH2

S

NHN

S

O

O

NH2

S

NHN

S

O

O

NH2

S

NHN

O

O

N

NH2

CH3

S

NHN

O

O

N

NH2

CH3

1. Sulfanilamide

2. Sulfadiazine

3. Sulfathiazole

4. Sulfamerazine

5. Sulfamethazine

6. Succinylsulfathiazole

EndStart

Minutes


Maprotiline HCL

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: 50 mM potassium phosphate pH 3.0/acetonitrile 65:35Flow rate: 1.0 mL/minInjection volume: 5 µL of 100 µg/mL maprotiline hydrochlorideDetection: UV @ 254 nm


1. Maprotiline HCL

Minutes


Meclizine HCL

HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 7.4mM sodium 1-heptanesulfonate in water/acetonitrile 58:42Flow rate: 1.0 mL/minInjection volume: 20 µL of 25 µg /mL sampleDetection: UV @ 230 nm


1. Meclizine HCL

Minutes


Methadone in Human Urine

%Recovery (%RSD) Compound n=3 n=9

(1 Subject) (3 Subject)(3 SPE Washes) (2 SPE Washes)

Methadone (0.5 µg/mL) 95.2 (1.0) 97.4 (3.0)

Methadone (0.1 µg/mL) 98.0 (4.8) 114.7 (8.2)

EDDP (0.2 µg/mL) 93.3 (1.0) 92.9 (2.4)

EDDP (0.4 µg/mL) 98.4 (2.9) 100.5 (5.8)

Estazolam (IS) 94.4 (3.3) 91.2 (91.2)

Chromatogram of Human Urine: A) Spiked Sample, B) Blank




Wash 12 mL 0.1M hydrochloric acid

Wash 22 mL methanol

Each elution diluted 1:1 with water for HPLC analysis

Elute2 mL 5% ammonium hydroxide

with 95% methanol

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ Guard Column, 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046980, Guard - WAT054225Mobile phase: 0.1% TFA in water/Methanol 60:40Flow rate: 1 mL/minInjection volume: 100 µL urine extractTemperature: 30˚ CDetection: UV @ 210 nm

Compounds:1. EDDP (0.2 µg/mL)2. Estazolam (I.S.) (0.2 µg/mL)3. Methadone (0.2 µg/mL)

No Conditioning

Optional Wash 32 mL of 5% ammonium hydroxide

with 60% methanol

AB

5 10 15

3

Minutes

1

2

0

0.01 AU

1. EDDP (Methadone Metabolite)

N+

CH3

CH3

CH3

3. Methadone

CH3

O

N

CH3

CH3

CH3

2. Estazolam

N

N

NN

Cl

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 20 mM potassium phosphate, pH 2.18/methanol 80:20Flow rate: 1.0 mL/minInjection volume: 15 µL of 200 µg/mLDetection: UV @ 254 nm


1. Methylphenidate HCL

Methylphenidate HCL

Minutes


HPLC Method

Column: SymmetryShield™ RP18, 4.6 x 250 mm, 5 µmPart number: 186000112Mobile phase: 1.92 g of 1-pentansulfonic acid sodium salt monohydrate,

0.27 g of sodium acetate trihydrate and 1.14 mL glacial acetic acid in 940 mL of water; 54% methanol/46% buffer



Metoprolol Tartrate and Oxprenolol

1. Metoprolol tartrate

2. Oxprenolol

Minutes


HPLC Method



Metronidazole (SymmetryShield™ RP18)

1. Metronidazole

Minutes


Metronidazole (Symmetry C18)

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: Water/Methanol 90:10Flow rate: 1.0 mL/minInjection volume: 10 µL of 100 µg/mL metronidazoleDetection: UV @ 254 nm

USP Tailing Factors:1. 1.2

1. Metronidazole

Minutes


Morphine and Its Glucuronide Metabolites in Serum

6

05

1

2

3

10

Minutes

15

mV

B

A




Morphine-D3-glucuronide 0.48 90.7 2.00.097 100 3.1

Morphine-D6-glucuronide 2.4 92.2 2.80.49 93.1 2.5

Morphine 3.6 102 3.60.73 102 3.2

HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µmPart number: WAT200655Mobile phase: 20 mM potassium phosphate, pH 6.4Flow rate: 1.0 mL/minInjection volume: 100 µL of porcine serum extractDetection: Fluorescence; ex 280 nm, em 355 nm

Compounds:1: Morphine-D3-glucuronide2: Morphine-D6-glucuronide3: Morphine

Condition1 mL methanol

Equilibrate1 mL water


Elute0.5 mL 3% triethylamine

No Evaporation

Sample injected directly


Wash1 mL water

3. Morphine

O

HO

ONCH3

H

OCOOH

OH

OHHO

1. Morphine-D3-glucuronide

HO

O H

NCH3

HO

2. Morphine-D6-glucuronide

OH

OH

COOHO O

ONCH3

H

HO

HO

Minutes


HPLC Method

Column: SymmetryShield™ RP18, 4.6 x 250 mm, 5 µmPart number: 186000112Mobile phase: Methanol/water 35:65, 2.93 g of sodium chloride,

1.0 mL of 0.1 N hydrochloric acidFlow rate: 1.0 mL/minInjection volume: 20 µLDetection: UV @ 220 nm


Nadolol

1. Nadolol

Minutes


HO

O

NOHO

HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µmPart number: WAT200655Mobile phase: 100 mM Ammonium acetate, pH 5.0/acetonitrile 88:12Flow rate: 1.0 mL/minInjection volume: 35 µL (500 µL eluate)Detection: UV @ 281 nm


Naltrexone

1. Naloxone (I.S.)

2. Naltrexone

Minutes


Naltrexone in Plasma


Naltrexone 3.3 108% 4.2%

HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µmPart number: WAT200655Mobile phase: 100 mM Ammonium acetate pH 5/acetonitrile 88:12Flow rate: 1.0 mL/minInjection volume: 1 mL spiked plasma with naloxone (I.S.)Temperature: 8˚ CDetection: UV @ 281 nm

Compounds:1. Naloxone (I.S.)2. Naltrexone


BA

0 2 4 6 8 10

0.001 AU

1

2

HO

O

NOHO

1. Naloxone (I.S.) 2. Naltrexone



Condition


Load

1 mL spiked plasma

with naloxone (I.S.)

Wash

1) 1 mL 5% methanol containing


2) 1 mL 20% methanol containing


Elute

0.5 mL of 25% methanol

containing 2% acetic acid


Not required

Minutes


Naltrexone in Plasma - LC/MS

CID mass spectra

Rela

tive

Abu

ndan

ce (%

)

Mass/Charge (m/z)

100 200 300 4000

0

324

324

100

A -H2 O

0

0

328

310100

B

-H2O

HO

O

NOHO

HO

O

NOHO



Loading1 mL of spiked plasma

Wash 11 mL of 5% methanol/


Wash 21 mL of 20% methanol/2% ammonium hydroxide

Elution0.5 mL 25% methanol/

1% acetic acid

Dilution0.5 mL water

HPLC Method

Column: Symmetry® C8, 2.1 x 30 mm, 5 µm Part number: WAT058977Mobile phase: 10 mM NH4OH, pH 5/Acetonitrile 88:12Flow rate: 200 µL/minInjection volume: 50 µL plasma extractMS: Micromass Quattro™ IIIon Source Temp: 120˚ CCID: 1.8e-3 mBar, 20 eVDesolvation Temp: 400 ˚CNebulizer: 40 L/hrDrying gas: 400 L/hrCone volt: 56 V

Conc Average % Std. Dev (RSD%) (rel. error)ng/mL n=8

0.5 0.6 0.09 16 15

1 0.9 0.06 6 -14

5 5.1 0.2 4 3

10 10.1 0.4 4 1

20 19.7 0.8 4 -2

50 49.1 3.9 8 -2

100 101.1 3.7 4 1

Coefficient of Determination: 0.996457Calibration Curve: 0.0508208* x + 0.00306776Response type: Internal Std (20 ng/mL Naloxone), Area * ( IS Conc. / IS Area)Curve type: Linear, Origin: Exclude, Weighting: 1x, Axis trans: None

Conc. (ng/mL)

0.0 50.0 100.00

5.35

Resp

onse

0 100

0.6HPLC-MS/MS (MRM Analysis at 0.5 ng/mL and 100 ng/mL

Naltrexone m/z 342 > 324Naloxone m/z 328 > 310

Analyte:Naltrexone

Int. Std.:Naloxone

0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80Time0

100

%

0

100

%

1.38

0.380.12 0.58 1.12 1.80

1.19

342.1>324.0

779

328.0>310.02.14e4

1.38

1.19

0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80Time0

100

%

0

100

%

1.34

1.17

100 ng/mL 342.1>324.08.90e4

328.0>310.02.42e4

1.34

1.17

0.5 ng/mL

0.5 1.0 1.5 2.00

1000

100

0

1000

100

Time (min)

A

B

C

D

Condition1 mL of methanol/1mL water


Naltrexone in Serum

1

2

B

A

0

0.05 AU

5 10 15

Minutes




Naltrexone 0.200 98% 3.2%

1.00 100% 3.5%

HPLC Method

Column: SymmetryShield™ RP8, 3.0 x 150 mm, 5 µmGuard Column: Sentry™ guard column, 3.9 x 20 mm, 5 µmPart numbers: Column - WAT094243, Guard - WAT200675Mobile phase: 20 mM ammonium acetate, pH 5/acetonitrile, 90:10Flow rate: 0.6 mL/minInjection volume: 20 µL of reconstituted porcine serum extractTemperature: 25˚ CDetection: UV @ 215 nm

Compounds:1: Naloxone (I.S.)2: Naltrexone


Load1 mL spiked porcine serumwith 0.2 µg naloxone (I.S.)


Elute1 mL methanol



1. Naloxone (I.S.)


HO

O

NOHO

2. Naltrexone

Minutes


Naproxen (Symmetry® C8)

HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 mm x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: Acetonitrile/water/glacial acetic acid 50:49:1Flow rate: 1.0 mL/minInjection volume: 5 µL of 100 µg/mL sampleDetection: UV @ 254 nm


1. Naproxen


Naproxen (SymmetryShield™ RP18)

HPLC Method

Column: SymmetryShield™ RP18, 4.6 x 250 mm, 5 µm Part number: 186000112Mobile phase: Acetonitrile/water 46:54, 2.0 mL of glacial acetic acid in 1 L of mobile phaseFlow rate: 1.0 mL/minInjection volume: 20 µLDetection: UV @ 254 nm


1. Naproxen

Minutes

2. Butyrophenone

OO


Nicergoline

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: Acetonitrile/100 mM sodium acetate, pH 5.0 40:60Flow rate: 1.0 mL/minInjection volume: 10 µL of 30 µg/mL nicergolineDetection: UV @ 227 nm


1. Nicergoline

Minutes


Nifedipine

HPLC Method



1. Nifedipine

Minutes


Oxycodone in Serum


Oxycodone 0.200 96.0% 6.4%

1.00 97.9% 1.0%

HPLC Method

Column: SymmetryShield™ RP8, 3 x 150 mm, 5 µmGuard Column: Sentry™ RP8, guard column, 3.9 x 20 mm, 5 µmPart Numbers: Column - WAT094243, Guard - WAT200675Mobile phase: 20 mM ammonium acetate, pH 5/acetonitrile, 90:10Flow rate: 0.6 mL/minInjection volume: 20 µL of reconstituted porcine serum extractTemperature: 25˚ CDetection: UV @ 215 nm

Compounds:1: Oxycodone2: Naltrexone (I.S.)

1. Oxycodone


H3CO

O

NCH3

OHO

2. Naltrexone (I.S.)

HO

O

NOHO

A

B

2

1

100 155Minutes

0.05 AU




Wash: 1 mL 5% methanol in water

Elute:1 mL methanol

Load:1 mL spiked porcine serum with

0.2 µg naloxone (I.S.)

Evaporate and Reconstitute:40˚ C under nitrogen stream,


Minutes


Oxytocin and Angiotensins in Serum


Oxytocin 5.0 103.7% 1.9%

Angiotensin I 5.0 97.8% 2.0%

Angiotensin II 5.0 99.2% 4.3%

HPLC Method

Column: SymmetryShield™ RP8, 4.6 x 100 mm, 3.5 µmGuard Column: Sentry™ guard column 3.9 x 20 mm, 3.5 µmPart numbers: Column - WAT094226, Guard - 186000704Mobile phase A: 0.1% TFA in water Mobile phase B: Acetonitrile/water 90:10 with 0.1% TFA

15 to 60% B in 22 minutesGradient: Time Profile

(min) %A %B0 85 1522 40 60

Flow rate: 1.4 mL/minInjection volume: 30 µL of reconstituted porcine extractTemperature: 30˚ CDetection: UV @ 214 nm

Compounds:1. Oxytocin2. Angiotensin II3. Angiotensin I (I.S.)

1

4 6 Minutes 8

0.05

2

3

B.

A.




Load1 mL spiked porcine serum with

20 µL of phosphoric acid

Wash1 mL 10% acetonitrile in 0.1% TFA

Elute1 mL acetonitrile/water 80:20

(with or without 0.1% TFA-no impact)


40 ˚C under nitrogen stream1 mL 0.1% aqueous TFA (for greater

sensitivity use less volume for reconstituting sample)

1. Oxytocin 2. Angiotensin II 3. Angiotensin I


Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: 20 mM ammonium acetate, pH 5.0/acetonitrile/methanol 50:40:10Flow rate: 1 mL/minInjection volume: 5 µL of 100 µg/mLDetection: UV @ 227 nm


1. Paclitaxel (Taxol)

Paclitaxel (Taxol)

Minutes


Paclitaxel (Taxol)- Resolution of Impurities

1. Paclitaxel (Taxol)

HPLC Method

Column: Symmetry® C18, 4.6 x 100 mm, 3.5 µmPart number: WAT066220Mobile phase: Water/acetonitrile/methanol 57:34:9Flow rate: 1.4 mL/minInjection volume: 25 µL of paclitaxel, 1 mg/mL in methanolDetection: UV @ 230 nm

Minutes


Papaverine HCL

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: 10 mM sodium phosphate pH 3.0, 2.88 g/L sodium lauryl sulfate/acetonitrile 50:50Flow rate: 1.0 mL/minInjection volume: 10 µL of 20 µg/mL papaverine hydrochlorideDetection: UV @ 254 nm


1. Papaverine HCL

Minutes


Paracetamol

HPLC Method



1. Paracetamol

Minutes


Paraquat and Diquat in Tap Water

2 64

1

2

PDA

(0.

08 A

UFS

)

257 nm

308 nm

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile Phase: 25 mM Octanesulfonate, pH 3.0/methanol 45:55Flow Rate: 0.75 mL/minInjection volume: 80 µLSample: 200 mL spiked tap water processed

on Oasis® MCX cartridgeDetection: PDA, 257 nm for Paraquat, 308 nm for Diquat

Oasis® MCX Method for QuaternaryAmines in Drinking Water

Conditions for Oasis® MCX Cartridge, 3 cc, 60 mgPart Number 186000254

Condition: 3 mL methanol

Rinse with 3 mL H2O

Load:

250 mL sample

Wash:

3 mL 50% methanol/ H2O

Elute: 2 mL of 1 M NH4CI

in 50% methanol/ H2O

For LC analysis dilute the eluent to 5 mL

with 50 mM sodium octanesulfonate

NN CH3CH3++

Compounds 2 mg/L Spike Level % Recovery, n=50.5 µg/L 2.0 µg/L

1. Paraquat 111 + 7 110 + 52. Diquat 91 + 4 96 + 4

1. Paraquat 2. Diquat

+

+N

N

Minutes


Peptides- Alberta Peptide Mixture

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase A: 0.1% TFA in water Mobile phase B: 0.1% TFA in acetonitrileGradient: Time Profile

(min) %A %B0 90 1030 60 4035 40 60

Flow rate: 0.8 mL/minInjection volume: 9 µL of peptide mixture; lyophilized sample dissolved in 1 mL mobile phaseTemperature: 35˚ CDetection: UV @ 214 nm

USP Tailing Factors1. 1.32. 1.23. 1.24. 1.25. 1.3

Peptides:Ac-Arg-Gly-x-x-Gly-Leu-Gly-Leu-Gly-Lys-amidewhere x-x=S1 Ala=Gly with free N alpha amino groupS2 Gly-GlyS3 Ala-GlyS4 Val-GlyS5 Val-Val

Minutes


Pharmaceutical Test Mix - 2.1 x 20 mm Intelligent Speed™ Separation

HPLC Method



Part numbers: Symmetry - 186002066SymmetryShield - 186002068

Mobile phase A: 0.1% HCOOH in Water Mobile phase B: 0.1% HCOOH in ACNGradient: Time Profile

(min) %A %B0 100 04 0 100

Flow rate: 0.6 mL/minInjection volume: 5 µLTemperature: 30˚ CDetection: UV @ 254 nm

5

81

2

3 710

9

4

6

0.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00

Minutes

0.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00

109

12

3

4

75 6

0.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00

Minutes

0.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00

8

SymmetryShield™ RP18, 3.5µm

Symmetry® C18, 3.5µm

t0 = 0.20 min

Max PSI = 1424

t0 = 0.20 min

Max PSI = 1224

NH

N

N

O

NH2N

O

HOH

HH

H

HO

H

Br

NH

N

N

O

NH2N

O

HOH

HH

H

HO

H

NH

N

N

O

NH2N

O

HOH

HH

H

HO

H

BrBr

NH

O

H3C O

F

HO

O

OH

OH

OH

H

H

O

F

HO

O

OH

OH

OH

H

H

O

HO

O

OH

OH

H H

H

O

HO

O

OH

OH

H H

H

NH2NH2

O

OH

O

H H

H

O

OH

O

H H

H

BrBr

5. 2-Amino-7-chlro-5-oxo-5H-[1]benzopyrano [2,3-b]pyridine-3 carbonitrile

8. 2-Bromofluorene

6. 6a-Methyl-17a-hydroxyprogesterone

2. Acetanilide

7. 3-Aminofluorathene

3. Triamcinolone

4. Hydrocortisone

1. 8-Bromoguanosine

10. Naptho(2,3-a)pyrene9. Perylene

Compounds:1. 8-Bromoguanosine2. Acetanilide3. Triamcinolone4. Hydrocortisone5. 2-Amino-7-chloro-5-oxo-5H-[1]

benzopyrano[2,3-b]pyridine-3-carbonitrile6. 6λMethyl-17λ-hydroxyprogesterone7. 3-Aminofluoranthene8. 2-Bromofluorene9. Perylene10. Naphtho(2,3-a)pyrene

Minutes

Minutes


Pharmaceutical Test Mix - 4.6 x 20 mm Intelligent Speed™ Separation

HPLC Method





(min) %A %B0 100 04 0 100




t0 = 0.17 min

Max PSI = 1122

t0 = 0.14 min

Max PSI = 1169

Minutes

0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50

1

7

2

3

4

5

6 89

10

Minutes

0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50

Minutes

0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50

Minutes

0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50

7

1

2

35

68

910

4

Minutes

0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50

Minutes

0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50

Compounds:1. 8-Bromoguanosine2. Acetanilide3. Triamcinolone4. Hydrocortisone5. 2-Amino-7-chloro-5-oxo-5H-[1]

benzopyrano[2,3-b]pyridine-3-carbonitrile6. 6λMethyl-17λ-hydroxyprogesterone7. 3-Aminofluoranthene8. 2-Bromofluorene9. Perylene10. Naphtho(2,3-a)pyrene

NH

N

N

O

NH2N

O

HOH

HH

H

HO

H

Br

NH

N

N

O

NH2N

O

HOH

HH

H

HO

H

NH

N

N

O

NH2N

O

HOH

HH

H

HO

H

BrBr

NH

O

H3C O

F

HO

O

OH

OH

OH

H

H

O

F

HO

O

OH

OH

OH

H

H

O

HO

O

OH

OH

H H

H

O

HO

O

OH

OH

H H

H

NH2NH2

O

OH

O

H H

H

O

OH

O

H H

H

BrBr

5. 2-Amino-7-chlro-5-oxo-5H-[1]benzopyrano [2,3-b]pyridine-3 carbonitrile

8. 2-Bromofluorene

6. 6a-Methyl-17a-hydroxyprogesterone

2. Acetanilide

7. 3-Aminofluorathene

3. Triamcinolone

4. Hydrocortisone

1. 8-Bromoguanosine

10. Naptho(2,3-a)pyrene9. Perylene

Minutes

Minutes


Phencyclidine in Human Urine

Compound % Recovery (n=6) %RSD (n=6) 0.3 µg/mL 1.5 µg/mL

Phencyclidine (PCP) 101.7 (2.3) 100.2 (0.8)

Ketamine (I.S.) 86.5 (1.0)

HPLC Method

Column: SymmetryShield™ RP18, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ Guard Column RP18, 3.9 x 20 mm, 5 µmPart numbers: Column - 186000108, Guard - 186000107Mobile phase: 50 mM Phosphate buffer, pH 7/Acetonitrile 70:30 Flow rate: 1 mL/minInjection volume: 20 µL urine extractTemperature: 30˚ CDetection: UV @ 210 nm (0.01 AUFS)

Compounds:1. Phencyclidine2. Ketamine HCI


Oasis® MCX Extraction MethodOasis® MCX Extraction Plate, 30 mg/96-well


Load

1 mL x 4 of acidified spiked human

urine (4 mL Total Sample)

Wash 1

1 mL 0.1N hydrochloric acid

Wash 2

1 mL methanol

Elute

1 mL 5% ammonium hydroxide

with 95% methanol

14

Minutes

0 7

1

2

B

A

0.01

AU

FS

N

1. Phencyclidine (PCP) 2. Ketamine (I.S.)

CH

CIO

3

NH

Minutes


Phenolics in Echinacea

HPLC Method

Column: Symmetry® C18, 4.6 x 250 mm, 5 µmPart number: WAT054275Mobile Phase A: 0.1% phosphoric acidMobile Phase B: AcetonitrileGradient: Time Profile

(min) %A %B0 90 1013 78 2240 60 40

Flow Rate: 1.5 mL/minInjection volume: 10 µLTemperature: 35° CDetection: UV @ 330 nm

Sample pre-preparation100 mg sample is extracted with 25 mL of ethanol:water (70:30)1 mL of the ethanolic extract is diluted 1:3 with water (~ pH 7)

• Recovery, measured with certified standards at 100 ppm in reagent water,was greater than 85 % for all compounds

• All analyses gave results within ± 35 % of the expected values with theexception of the liquid supplement (see goldenseal analysis)

• The selective SPE extraction and cleanup procedure provided a convenientanalysis of echinacea phenolics in complex matrix such as in herbal tea

Oasis® MAX method for phenolics in echinaceaConditions for Oasis® MAX Cartridge, 3 cc, 60 mg


Condition/Equilibrate:1 mL methanol/1 mL water

Load:3 mL of diluted sample

Wash 1:2 mL of 50 mM sodium acetate

Wash 2:2 mL of methanol

Dry Cartridge:air dry for 15 min with vacuum

Elute:3 mL MTBE/methanol/TFA (49:49:2)

Evaporate and Reconstitute:1 mL mobile phase

1

2

3

Tea bagextract

Minutes10 200

1. cafteric acid2. chlorogenic acid3. cichoric acidtotal: 5 mg / teabag

Herbal tea extractbefore SPE cleanup

Herbal tea extract after SPE cleanupusing Oasis® MAX

Minutes


Prednisone

HPLC Method

Column: SymmetryShield™ RP18, 4.6 x 150 mm, 5 µmPart number: 18600109Mobile phase: 20 mM Phosphate buffer, pH 7/Acetonitrile 65:35 Flow rate: 1.0 mL/minInjection volume: 5 µLDetection: UV @ 254 nm


1. Prednisone

Minutes


Procainamide in Serum


Procainamide 0.100 93.8% 1.8%0.500 98.1% 2.1%

HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ guard column, 3.9 x 20 mm, 5 µmPart numbers: Column - WAT200655, Guard - WAT200675Mobile phase: 20 mM potassium phosphate, pH 3.0/methanol 97:3Flow rate: 1.0 mL/minInjection volume: 50 µL of reconstituted porcine serum extractTemperature: 30˚ CDetection: UV @ 220 nm

Compounds:1: Procainamide2: Sulfanilamide (I.S.)

1. Procainamide


O

NH2 2 3

2 3

H NN

CH CH

CH CH

2. Sulfanilamide






Elute1 mL methanol


40 ˚C under nitrogen stream200 µL of 50 µg/mL sulfanilamide (I.S.)

in water

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 50 mM potassium phosphate, pH 3.0/methanol 85:15Flow rate: 1.0 mL/minInjection volume: 10 µL of 40 µg/mL sampleDetection: UV @ 254 nm


1. Procainamide

2. N-Acetylprocainamide

3. N-Propionylprocainamide

Procainamides at pH 3.0

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µmPart number: WAT046970Mobile phase: 20 mM potassium phosphate, pH 6.0/acetonirtrile 90:10Flow rate: 1.0 mL/minInjection volume: 10 µL of 40 µg/mL each compoundDetection: UV @ 254 nm


1. Procainamide

2. N-Acetylprocainamide

3. N-Propionylprocainamide

Procainamides at pH 6.0

Minutes


Prochlorperazine - Isolation of Degradation Products,Transfer from Analytical to Prep

HPLC Method

Columns: A. Symmetry® C18, 3.9 x 150 mm, 5 µmB. SymmetryPrep™ C18, 7.8 x 150 mm, 7 µm

Part numbers: A. WAT046980, B. WAT066288Mobile phase A: 0.1% TFA in Water Mobile phase B: AcetonitrileGradient: Time Profile

(min) %A %B0 90 1050 40 60

Flow rate: A. 0.7 mL/min B. 2.8 mL/minInjection volume: Prochlorperazine edisylate

A. 0.8 mg B. 3.2mgDetection: UV @ 280 nm

1. Prochlorperazine Edisylate

1. Symmetry® C18 , 5 µm, 3.9 mm x 150 mm

2. SymmetryPrep™ C18 , 7 µm, 7.8 mm x 150 mm

Minutes


Profens (Gradient)-4.6x 20mm Intelligent Speed™ Separation

HPLC Method





(min) %A %B0 65 352 60 40


Compounds:1. Ketoprofen2. Fenoprofen3. Flurbiprofen4. Ibuprofen


t0 = 0.19 min

Max PSI = 1090

13

2

4

0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.000.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00

2

31

4

0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.000.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00


t0 = 0.15 minMax PSI = 1111

Minutes

Minutes

O

O

OH

CH3O

O

OH

CH3

O

O OH

CH3

O

O OH

CH3

O

F

OH

CH3

O

F

OH

CH3

O

OH

CH3

CH3

CH3

O

OH

CH3

CH3

CH3

1. Ketoprofen

2. Fenoprofen

3. Flurbiprofen

4. Ibuprofen


3

1

2

4

0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.000.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00

Profens (Isocratic) - 4.6 x 20 mm Intelligent Speed Separation

HPLC Method




Mobile phase A: 0.1% HCOOH in Water Mobile phase B: 0.1% HCOOH in ACNIsocratic: 65% A, 35% BFlow rate: 3.0 mL/minInjection volume: 10 µLTemperature: 30˚ CDetection: UV @ 220 nm

Compounds:1. Ketoprofen2. Fenoprofen3. Flurbiprofen4. Ibuprofen


t0 = 0.18 min

Max PSI = 1082


t0 = 0.15 min

Max PSI = 1111

Minutes

1

2

43

0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00

Minutes

O

O

OH

CH3O

O

OH

CH3

O

O OH

CH3

O

O OH

CH3

O

F

OH

CH3

O

F

OH

CH3

O

OH

CH3

CH3

CH3

O

OH

CH3

CH3

CH3

1. Ketoprofen

2. Fenoprofen

3. Flurbiprofen

4. Ibuprofen


Promethazine- Impurities Profile

HPLC Method

Column: SymmetryShield™ RP18, 3.0 x 150 mm, 5 µmPart number: 186000692Mobile phase A: 20 mM potassium phosphate, pH 7.0Mobile phase B: AcetonitrileGradient: Time Profile

(min) %A %B0 95 530 20 80

Flow rate: 1.0 mL/minInjection volume: 10 µL of 0.5 mg/mLDetection: UV @ 254 nm

1. Promethazine HCL

Minutes


Propranolol in Human Urine

Compound %Recovery (%RSD) 0.08 µg/mL 0.4 µg/mL

Propranolol (n=3) 105.8 (2.7) 98.5 (0.7)

Metoprolol (n=3) 101.0 (3.4) 99.6 (0.4)

Propranolol Interday (n=6) 99.0 (0.9)

Propranolol Interperson (n=9) 100.4 (6.4)

Metoprolol Interday (n=6) 100.3 (0.9)

Metoprolol Interperson (n=9) 97.3 (2.6)

Oxprenolol (I.S.) 91.1 (3.2)


HPLC Method

Column: SymmetryShield™ RP18, 3.9 x 150 mm, 5 µmGuard Column: SymmetryShield™ RP18, 3.9 x 20 mm, 5 µmPart numbers: Column - 186000108, Guard - 186000107 Mobile phase: 0.1% TFA in water/Acetonitrile 80:20Flow rate: 1 mL/minInjection volume: 50 µL Temperature: 30˚ CDetection: UV @ 275 nm

Compounds: 1. Metoprolol2. Oxprenolol (I.S.)3. Propranolol




Wash 12 mL 0.1M hydrochloric acid

Wash 22 mL of 100% methanol

Elute2 mL 95% methanol with 5% ammonium hydroxide

Neutralize each elution with 100 µL of acetic acid. Evaporate une N2 at 40 ˚C andreconstitute with 300 µL of water

Wash 32 mL of 50% methanol with 5% ammonium hydroxide

No Conditioning

1

23

4 8 12 160

Minutes

AB

0.00

80 A

UFS

2. Oxprenolol (I.S.)

O

OCH2

HN CH3

CH3

3. Propranolol

O

OH

NH

CH3

CH3

1. Metoprolol

O

OHHN CH3

CH3H3CO

Minutes


Propranolol in Serum

1

2

A

B

0

Minutes

124 8

0.002 AU

Oasis® HLB Extraction MethodOasis® HLB 1 cc/30mg Extraction

CartridgePart Number WAT094225


Propranolol 0.800 85.9% 2.1%4.00 96.4% 2.4%

HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ guard column, 3.9 x 20 mm, 5 µmPart numbers: Column - WAT200655, Guard - WAT200675Mobile phase: 20 mM potassium phosphate, pH 7/methanol 38:62Flow rate: 1.0 mL/minInjection volume: 20 µL of reconstituted porcine serum extractTemperature: 30˚ CDetection: UV @ 254 nm

Compounds:1: Propranolol2: Butyl paraben (I.S.)

O

OHNH




Elute1 mL methanol with 5 µg

butyl paraben


40 ˚C under nitrogen stream200 µL methanol

1. Propranolol


Minutes

2. Butyl paraben (I.S.)


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 50mM potassium phosphate, pH 3.0/acetonitrile 85:15Flow rate: 1.0 mL/minInjection volume: 5 µL of 2.88 µg/mL sampleDetection: UV @ 261 nm


1. Pseudoephedrine HCL

Pseudoephedrine HCL

Minutes


Pseudoephedrine HCL and Chlorpheniramine

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046970Mobile phase A: 50 mM potassium phosphate, pH 3.0Mobile phase B: AcetonitrileGradient: Time Profile

(min) %A %B0 85 151 85 1515 50 50

Flow rate: 1.0 mL/minInjection volume: 5 µL of 1.8 mg/mL pseudoephedrine and 120 µg/mL chlorpheniramine sampleDetection: UV @ 261 nm


2. Chlorpheniramine Maleate


Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase A: 50 mM potassium phosphate, pH 3.0Mobile phase B: AcetonitrileGradient: Time Profile

(min) %A %B0 85 151 85 1515 50 50

Flow rate: 1.0 mL/minInjection volume: 5 µL of 2.88 µg/mL pseudoephedrine and 120 µg/mL triprolidine extracted tablet sampleDetection: UV @ 261 nm



Pseudoephedrine HCL and Triprolidine HCL

2. Triprolidine HCL

Minutes


Pseudoephedrine HCL and Codeine

HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µmPart Number: WAT200655Mobile phase A: 50 mM potassium phosphate, pH7Mobile phase B: Acetonitrile Gradient: Time Profile

(min) %A %B0 85 1515 50 50

Flow rate: 1 mL/minInjection Volume: 5 µL of 2 mg/mL pseudoephedrine HCL and 0.2 mg/mL codeineDetection: UV @ 254 nm



2. Codeine

Minutes


Purine Alkaloids




Theobromine 0.100 103.0% 3.4%0.500 104.0% 2.4%

Paraxanthine 0.100 101.0% 6.2%0.500 98.9% 2.3%

Theophylline 0.100 100.0% 5.2%0.500 101.0% 2.1%

Caffeine 0.100 92.6% 4.4%0.500 97.5% 3.2%

HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ guard column, 3.9 x 20 mm, 5 µmPart Numbers: Column - WAT094243, Guard - WAT200675Mobile phase: 20 mM ammonium acetate, pH 5/acetonitrile, 95:5Flow rate: 0.6 mL/minTemperature: 25˚ CInjection volume: 20 µL of reconstituted porcine serum extract Detection: UV @ 273 nm

Compounds:1: Theobromine2: Paraxanthine3: Theophylline4: b-hydroxyethyltheophylline (I.S.)5: Caffeine


Load1 mL porcine serum with 0.2 µgß-hydroxyethyltheophylline (I.S.)

Wash1 mL water

Elute1 mL methanol



1. Theobromine


3. Theophylline2. Paraxanthine

4. ß-hydroxyethyltheophylline (I.S.)

N

N N

N

O

O CH2CH2OH

H3C

CH3

5. Caffeine

N

N N

N

O

O CH2

H3C

CH3

B

A

0.03 AU

0 5 10 15

1

2

3

4

5


Quinidine Sulfate and Related Substance

HPLC Method

Column: SymmetryShield™ RP18, 4.6 x 250 mm, 5 µmPart Number: 186000112Mobile phase: 860 mL water, 20 mL methanesulfonic acid sloution, 20 mL diethylamine solution,

100 mL acetonitrile; pH adjusted to 2.6 with diethylamine solutionDiethylamine solution: 10 mL diethylamine in 100 mL water Methanesulfonic acid solution: 14 mL methanesulfonic acid and 8 mL glacial acetic acid in 200 mL water

Flow rate: 1.0 mL/minInjection volume: 50 µL Detection: UV @ 235 nm

USP Tailing Factor1. 1.762. 1.33

1. Quinidine sulfate

2. Dihydroquinidine sulfate

Minutes


Ranitidine (SymmetryShield™ RP18)

HPLC Method

Column: SymmetryShield™ RP18, 4.6 x 150 mm, 5 µmPart Number: 18600109Mobile phase: 20 mM phosphate buffer, pH 7.0/acetonitrile, 85:15Flow rate: 1.0 mL/minInjection volume: 5 µLDetection: UV @ 254 nm


1. Ranitidine

1

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 100 mM sodium acetate, 5mM camphosulfonic acid, pH 6.2/ acetonitrile/methanol 80:10:10Flow rate: 1.0 mL/minInjection volume: 5 µL of 100 µg/ml sampleDetection: UV @ 254 nm


1. Ranitidine

Ranitidine (Symmetry® C8)

Minutes


Ranitidine in Serum




Ranitidine 0.100 104% 1.9%

0.500 102% 1.7%

HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ guard column, 3.9 x 20 mm, 5 µmPart numbers: Column - WAT200655, Guard - WAT200675Mobile phase: 20 mM potassium phosphate, pH 3.0/methanol 97:3Flow rate: 1.0 mL/minInjection volume: 50 µL of reconstituted porcine serum extractTemperature: 30˚ CDetection: UV @ 220 nm

Compounds:1: Sulfanilamide (I.S.)2: Ranitidine




Elute1 mL methanol


40 ˚C under nitrogen stream200 µL of 50 µg/mL sulfanilamide (I.S.)

in water


O

S

HN

HN

CH3

CHNO2

N

H3C

H3C

2. Ranitidine1. Sulfanilamide

Minutes


Salicylic Acid and Related Compoundsin Serum




Benzoic Acid 0.100 84.8% 3.8%0.500 87.1% 3.0%

Salicylic Acid 0.100 92.3% 5.0%0.500 91.3% 3.3%

HPLC Method

Column: SymmetryShield™ RP8, 3.0 x 150 mm, 5 µmGuard Column: Sentry™ guard column, 3.9 x 20 mm, 5 µmPart numbers: Column - WAT094243, Guard - WAT200675Mobile phase: 1.2% glacial acetic acid/acetonitrile 75:25Flow rate: 0.6 mL/minInjection volume: 10 µL of reconstituted porcine serum extractTemperature: 40˚ CDetection: UV @ 236 nm

Compounds:1: Benzoic acid2: Nalidixic acid (I.S.)3: Salicylic acid



acidified with 20 µL phosphoric acid


Elute1 mL methanol


40 ˚C under nitrogen stream1 mL 5 µg/mL nalidixic acid

in mobile phase

1. Benzoic acid


2. Nalidixic acid (I.S.)

1

2

3

B

A

0

0.035 AU

5 10 15Minutes

3. Salicylic acid

Minutes


Salicylic Acid and Related Compounds

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: 50 mM potassium phosphate pH 3.0/acetonitrile 70:30Temperature: 40˚ CFlow rate: 0.7 mL/minInjection volume: 6 µL of phthalic acid (0.5 mg/mL), benzoic and salicylic acids (1 mg/mL)Detection: UV @ 254 nm


2. Salicylic Acid

1. Phthalic Acid

3. Benzoic Acid

Minutes


Speed Mix - 2.1 x 20 mm Intelligent Speed™ Separation

HPLC Method





(min) %A %B0 100 04 0 100



t0 = 0.17 minMax PSI = 1452


t0 = 0.17 minMax PSI = 1247

1

2

3

4

5

6

7

89

1110

0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.000.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00

1

2

3

4

56

7

89 1110

0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.000.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00

Compounds:1. Theophylline2. 2-Acetylfuran3. Acetanilide4. Acetophenone5. Propiophenone6. Butyrophenone7. Benzophenone8. Valerophenone9. Hexanophenone10. Heptanophenone11. Octanophenone

O

O

O

O

O

CH3

O

CH3

OO

OO

NH

O

H3C

OO

OO

1. Theophylline 2. 2-Acetylfuran

4. Aceophenone

3. Acetanilide

5. Propiophenone 6. Butyrophenone

8. Valerophenone7. Benzophenone

OO

9. Hexanophenone

OO

10. Heptanophenone

OO

11. Octanophenone

Minutes

Minutes


Speed Mix - 4.6 x 20 mm Intelligent Speed™ Separation

HPLC Method





(min) %A %B0 100 04 0 100



t0 = 0.16 min

Max PSI = 1124


t0 = 0.15 min

Max PSI = 1162

34

68

910

111

5

2

7

0.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.000.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00

7

1

2

3

4

56 8 9

1011

0.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.000.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00

Compounds:1. Theophylline2. 2-Acetylfuran3. Acetanilide4. Acetophenone5. Propiophenone6. Butyrophenone7. Benzophenone8. Valerophenone9. Hexanophenone10. Heptanophenone11. Octanophenone

O

O

O

O

O

CH3

O

CH3

OO

OO

NH

O

H3C

OO

OO

1. Theophylline 2. 2-Acetylfuran

4. Aceophenone

3. Acetanilide

5. Propiophenone 6. Butyrophenone

8. Valerophenone7. Benzophenone

OO

9. Hexanophenone

OO

10. Heptanophenone

OO

11. Octanophenone

Minutes

Minutes


HPLC Method

Column: Symmetry® C8 ,3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: Acetonitrile/water 50:50Flow rate: 1.0mL/minInjection volume: 5µL of 10 µg/mL sampleDetection: UV @ 254nm


1. Prednisolone

Steroids

Vo: Uracil

2. Betamethasone

3. Prednisolone Acetate

4. Betamethasone Valerate

Minutes


Steroids in Serum

0 4 8 12 16Minutes

BA

12 3

4

0.05 AU




Prednisolone 1.00 93.8% 4.7%5.00 92.0% 1.4%

Betamethasone 1.00 85.7% 2.3%5.00 91.3% 1.5%

Betamethasone 4.00 95.4% 2.2%

Valerate 20.00 90.6% 1.3%

HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ guard column, 3.9 x 20 mm, 5 µmPart numbers: Column - WAT200655, Guard - WAT200675Mobile phase: 20 mM potassium phosphate, pH 7/methanol 41:59Flow rate: 1.0 mL/minInjection volume: 5 µL of reconstituted porcine serum extractDetection: UV @ 254 nm

Compounds:1: Prednisolone2: Betamethasone3: Butyl Paraben (I.S.)4: Betamethasone Valerate




Elute1 mL methanol, added 50 µL of 0.1 mg/mL butyl paraben (I.S.)


200 µL acetonitrile

4. Betamethasone valerate


1. Prednisolone 2. Betamethasone 3. Butyl Paraben (I.S.)

Minutes


Steroids - 2.1 x 20 mm Intelligent Speed™ Separation

HPLC Method

Column: Symmetry® C18, 2.1 x 20 mm, 3.5 µm IS™

Part number: 186002066Mobile phase A: Water Mobile phase B: ACNGradient: Time Profile

(min) %A %B0 80 204 36 64


t0 = 0.33 min

Max PSI = 1280

6

2 34 5

0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.000.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00

1

1. Prednisolone 2. Cortisone

O

O

O

OH

CH3

CH3

OH

H

H H

O

O

O

OH

CH3

CH3

OH

H

H H

3. Corticosterone

O

O

CH3OH

CH3

OH

H

H

H

O

O

CH3OH

CH3

OH

H

H

H

4. Estradiol

CH3OH

OH

H

H H

CH3OH

OH

H

H H

5. Estrone

OCH3

OH

H

H

H

OCH3

OH

H

H

H

6. Progesterone

O

O

CH3

CH3

CH3

H

H

H

O

O

CH3

CH3

CH3

H

H

H

Minutes

Symmetry® C18, 3.5µmCompounds:1. Prednisolone2. Cortisone3. Corticosterone4. Estradiol5. Estrone6. Progesterone


Steroids - 4.6 x 20 mm Intelligent Speed™ Separation

HPLC Method




Mobile phase A: Water Mobile phase B: ACNGradient: Time Profile

(min) %A %B0 80 204 36 64



t0 = 0.14 min

Max PSI = 1190


t0 = 0.14 min

Max PSI = 1132

Minutes

Minutes

12 3

45

6

0.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.000.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00

1

4

2 35

6

0.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.000.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00

Compounds1. Prednisone2. Cortisone3. Corticosterone4. Estradiol5. Estrone6. Progesterone

1. Prednisolone 2. Cortisone

O

O

O

OH

CH3

CH3

OH

H

H H

O

O

O

OH

CH3

CH3

OH

H

H H

3. Corticosterone

O

O

CH3OH

CH3

OH

H

H

H

O

O

CH3OH

CH3

OH

H

H

H

4. Estradiol

CH3OH

OH

H

H H

CH3OH

OH

H

H H

5. Estrone

OCH3

OH

H

H

H

OCH3

OH

H

H

H

6. Progesterone

O

O

CH3

CH3

CH3

H

H

H

O

O

CH3

CH3

CH3

H

H

H


Succinimides

HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 100 mM potassium phosphate, pH 6.9/methanol/water 20:30:50Flow rate: 1.0 mL/minInjection volume: 10 µL of 40-500µg/mL sampleDetection: UV @ 214 nm


1. Ethosuximide

2. Phensuximide

3. Methsuximide

Minutes

1

2

3


Sulfa Drugs

HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5µmGuard Column: Sentry™ Guard Column 3.9 x 20 mm, 5µmPart numbers: Column - WAt046970, Guard - WAT054250Mobile phase: Water/methanol/glacial acetic acid 79:20:1Flow rate: 1.0 mL/minInjection volume: 10 µL of sample with components at 10 to 39 µg/mLDetection: UV @ 254 nm

USP Tailing Factors1. 1.272. 1.193. 1.184. 1.155. 1.126. 1.11

1. Sulfanilamide

SNH

O

O

N

N

NH2SNH

O

O

N

N

NH2

2. Sulfadiazine

S

NHN

S

O

O

NH2

S

NHN

S

O

O

NH2

3. Sulfathiazole

S

NHN

O

O

N

NH2

CH3

S

NHN

O

O

N

NH2

CH3

4. Sulfamerazine

5. Sulfamethazine 6. Succinylsulfathiazole


Sulfa Drugs in Serum




Sulfadiazine 2.00 98.4% 2.7%10.0 96.9% 0.65%

Sulfamerazine 2.00 93.5% 1.9%10.0 96.4% 0.74%

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: 1% glacial acetic acid and 4% methanol in waterFlow rate: 1.0 mL/minInjection volume: 10 µL of reconstituted porcine serum extractTemperature: 25˚ CDetection: UV @ 254 nm

Compounds:1: Sulfadiazine2: Sulfathiazole (I.S.)3. Sulfamerazine

SNH

O

O

N

N

NH2SNH

O

O

N

N

NH2

Condition


Load

1 mL spiked porcine serum

with 10 µg/mL sulfathiazole (I.S.),

20 µL phosphoric acid

Wash

1 mL 5% methanol in water

Elute

1 mL methanol


40 ˚C under nitrogen stream

1 mL mobile phase

1. Sulfadiazine


S

NHN

S

O

O

NH2

S

NHN

S

O

O

NH2

2. Sulfathiazole (I.S.)

S

NHN

O

O

N

NH2

CH3

S

NHN

O

O

N

NH2

CH3

3. Sulfamerazine

0.004 AU

B

A

15105

23

1

MinutesMinutes


Sulfa Drugs - 2.1 x 20 mm Intelligent Speed™ Separation

HPLC Method


Part number: 186002066Mobile phase A: 0.1% HCOOH in Water Mobile phase B: 0.1% HCOOH in MeOHGradient: Time Profile

(min) %A %B0 100 04 50 50


Compounds:1. Sulfadiazine2. Sulfathiazole3. Sulfamerazine4. Sulfadimidine5. Sulfamethoxazole6. Sulfisoxazole7. Sulfadimethoxine


t0 = 0.17 min

Max PSI = 2050

Minutes

0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.000.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00

1

32

4

5

6 7

SNH

O

O

N

N

NH2SNH

O

O

N

N

NH2

1. Sulfadiazine

S

NHN

O

O

N

NH2

CH3

S

NHN

O

O

N

NH2

CH3

3. Sulfamerazine

S

NHN

S

O

O

NH2

S

NHN

S

O

O

NH2

2. Sulfathiazole

S

NHN

N

O

O

NH2

CH3

CH3

S

NHN

N

O

O

NH2

CH3

CH3

4. Sulfadimidine

S

NHN

OO

O

NH2CH3

S

NHN

OO

O

NH2CH3

5. Sulfamethoxazole

SNH

N

O

O

O

CH3 NH2

CH3

SNH

N

O

O

O

CH3 NH2

CH3

6. Sulfisoxazole

S

NH

NN

O

O

O

O

NH2

CH3

CH3 S

NH

NN

O

O

O

O

NH2

CH3

CH3

7. Sulfadimethoxine


Sulfa Drugs -4.6 x 20 mm Intelligent Speed™ Separation

HPLC Method


Part number: 186002090Mobile phase A: 0.1% HCOOH in Water Mobile phase B: 0.1% HCOOH in MeOHGradient: Time Profile

(min) %A %B0 100 04 50 50


Compounds:1. Sulfadiazine2. Sulfathiazole3. Sulfamerazine4. Sulfadimidine5. Sulfamethoxazole6. Sulfisoxazole7. Sulfadimethoxine


t0 = 0.15 min

Max PSI = 2280

Minutes

0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.000.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00

53

1

4

26 7

SNH

O

O

N

N

NH2SNH

O

O

N

N

NH2

1. Sulfadiazine

S

NHN

O

O

N

NH2

CH3

S

NHN

O

O

N

NH2

CH3

3. Sulfamerazine

S

NHN

S

O

O

NH2

S

NHN

S

O

O

NH2

2. Sulfathiazole

S

NHN

N

O

O

NH2

CH3

CH3

S

NHN

N

O

O

NH2

CH3

CH3

4. Sulfadimidine

S

NHN

OO

O

NH2CH3

S

NHN

OO

O

NH2CH3

5. Sulfamethoxazole

SNH

N

O

O

O

CH3 NH2

CH3

SNH

N

O

O

O

CH3 NH2

CH3

6. Sulfisoxazole

S

NH

NN

O

O

O

O

NH2

CH3

CH3 S

NH

NN

O

O

O

O

NH2

CH3

CH3

7. Sulfadimethoxine


Sulfamethoxazole and Trimethoprim

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: Water/methanol/glacial acetic acid 79:20:1Flow rate: 1.0 mL/minInjection volume: 10 µL of 100 µg/mL sulfamethoxazole and 30 µg/mL trimethroprimDetection: UV @ 254 nm


1. Trimethoprim

2. Sulfamethoxazole

Minutes


Sulfamethoxazole and Trimethoprimin Serum




Sulfamethoxazole 1.20 90.4% 1.3%0.240 95.4% 3.4%

Trimethoprim 1.50 96.7% 1.1%0.300 99.3% 3.2%

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ guard column, 3.9 x 20 mm, 5 µm Part number: Column - WAT046980Mobile phase: 25 mM ammonium acetate, pH 5/methanol 82:18 (v/v)Flow rate: 1.0 mL/minInjection volume: 20 µL of reconstituted porcine serum extractDetection: UV @ 290 nm

Compounds:1: Sulfamerazine (I.S.)2: Trimethoprim3: Sulfamethoxazole



with 20 µL phosphoric acid and2.5 µg/mL sulfamerazine (I.S.)


Elute1 mL methanol



1. Sulfamerazine (I.S.)

` 5 10 15 20Minutes

00.02 AU


B.

A.

1

2

2. Trimethoprim 3. Sulfamethoxazole

3


Symmetry® C18 pH 3 Batch Test

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: 50 mM potassium phosphate pH 3.0/acetonitrile 80:20Flow rate: 1.0 mL/minInjection volume: 20 µL of mixture with chlorpheniramine, maleate, toluamide and propranololDetection: UV @ 230 nm

Compounds1. Maleate2. Toluamide3. Chlorpheniramine4. Propranolol

O

OH

NH

CH3

CH3

1. Maleate

2. Toluamide

3. Chlorpheniramine

4. Propranolol

Minutes


Synthetic Antibiotics

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: 0.1% phosphoric acid in water/methanol 62:38Flow rate: 1.0 mL/minInjection volume: 10 µL of mixture with 30 µg/mL furazolidone and oxolinic acid and 100 µg/mL nolidixic acidDetection: UV @ 254 nm


1. Furazolidone

2. Oxolinic Acid

3. Nalidixic Acid

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µmPart number: WAT046970Mobile phase: 50 mM potassium phosphate, pH 3/acetonitrile 55:45Flow rate: 1.0 mL/minInjection volume: 5 µL of 100 µg/mL Detection: UV @ 254 nm


Tamoxifen

1. Tamoxifen Citrate

Minutes


Tamoxifen- Isolation of Impurities, Transfer from Analytical to Prep

HPLC Method

Columns: Symmetry® C18, 3.0 x 150 mm, 5 µmSymmetryPrep™ C18, 7.8 x 300 mm, 7 µm

Part numbers: Symmetry - WAT054200SymmetryPrep - WAT066235

Mobile phase: Acetonitrile/50 mM potassium phosphate buffer, pH 3.0 40:60Flow rate: A. 0.4 mL/min B. 5.6 mL/minInjection volume: 5 mg/mL tamoxifen citrate

A. 15 mg B. 101mgDetection: UV @ 254 nm

1. Tamoxifen Citrate

1. Symmetry® C18 , 5 µm, 3.0 mm x 150 mm

1

1. SymmetryPrep™ C18 , 7 µm, 7.8 mm x 300 mm

Minutes


HPLC Method

Column: SymmetryShield™ RP18, 4.6 x 150 mm, 5 µmPart number: 186000109Mobile phase: 20 mM phosphate buffer, pH 7.0/acetonitrile 25:75Flow rate: 1.0 mL/minInjection volume: 5 µL Detection: UV @ 220 nm


Terfenadine

1. Terfenadine

Minutes


HPLC Method

Column: Symmetry® C8, 4.6 x 250 mm, 5 µmPart number: WAT054270Mobile phase: 100 mM triethylammonium phosphate, pH 7.0/methanol 20:80Flow rate: 1.0 mL/minInjection volume: A. 15 µL of mixture with 0.6 mg/mL terfenadine and 0.15 mg/mL

of terfenadine related compound ARSB.15 µL of 8mg/mL crushed tablet ( equivalent to 0.6mg/mL terfenadine)

Detection: UV @ 235 nm

Compounds:1. Terfenadine2. Terfenadine Related Compound ARS


1. Terfenadine

Terfenadine and Related Compound

Tablet:

Standard:

Minutes


Testosterone Esters in Serum

Oasis® HLB Extraction MethodOasis

®HLB 1 cc/30 mg Extraction Cartridge



Testosterone 1.00 98% 1.2%Acetate 0.200 94% 3.7%

Testosterone 1.00 100% 1.9%Propionate 0.200 94% 4.3%

Testosterone 1.00 94% 1.6%Benzoate 0.200 87% 3.2%

HPLC Method

Column: Symmetry® C8, 4.6 x 75 mm, 3.5 µmGuard Column: Sentry™ guard column, 3.9 x 20 mm, 5 µmPart Numbers: Column - WAT066224, Guard - WAT064225Mobile phase: Acetonitrile/water 60:40Flow rate: 1.5 mL/minInjection Volume: 20 µL of reconstituted porcine serum extractDetection: UV @ 254 nm

Compounds:1: Testosterone acetate2: Testosterone propionate3: Testosterone benzoate4: Testosterone enanthate (I.S.)


Load1 mL sample with 800 µL spiked porcine

serum and 200 µL of methanol


Elute1 mL methylene chloride: methanol 50:50 (v/v)


500 µL methanol with 5 µg/mL of testosterone enanthate

3. Testosterone benzoate


1. Testosterone acetate 2. Testosterone propionate 4. Testosterone enanthate (I.S.)

Minutes0 10 20

1

2

34

B

A

0.008 AU

Minutes


Tetracyclines

HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 10 mM sodium phosphate, pH 6.25/methanol 45:55Flow rate: 1.0 mL/minInjection volume: 20 µL of 500 µg/mL sampleDetection: UV @ 280 nm


1. Doxycycline

2. Minocycline

3. Tetracycline

Minutes


Tetracyclines in Serum

10

0.006

3

2

1

20 30

B

A




Minocycline 2.50 96.1% 1.3%0.500 88.0% 1.6%

Tetracycline 2.50 101.0% 0.5%0.500 97.8% 1.4%

HPLC Method

Column: SymmetryShield™ RP8, 3.0 x 150 mm, 5 µmGuard Column: Sentry™ guard column, 3.9 x 20 mm, 5µmPart numbers: Column - WAT094243, Guard - WAT200675Mobile phase: 0.1% TFA in Water, Methanol, Acetonitrile 91:2:7Flow rate: 0.90 mL/minInjection volume: 20 µL of reconstituted porcine serum extractDetection: UV @ 350 nm

Compounds:1: Minocycline2: Tetracycline3: Demeclocycline (I.S.)



with 20 µL phosphoric acid and5.0 µg/mL demeclocycline (I.S.)


Elute1 mL methanol



2. Tetracycline


1. Minocycline 3. Demeclocycline (I.S.)

Minutes


Theophylline and Related Compounds

HPLC Method

Column: SymmetryShield™ RP18, 3.0 x 150 mm, 5 µmPart number: 186000692Mobile phase: 5 mM potassium phosphate, pH 2.0/acetonitrile 95:5Flow rate: 0.6 mL/minInjection volume: 5 µL injection of solution containing theobromine (0.22 mg/mL),

theophylline (0.26 mg/mL), and 7-(2-hydroxyethyl) theophylline (0.13 mg/mL)Detection: UV @ 270 nm

1. Theobromine

2. Theophylline

3. 7-(2-hydroxyethyl) Theophylline

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ Guard Column 3.9 x 20mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 10 mM potassium phosphate, pH7.0/ methanol 76:24Flow rate: 1.0 mL/minInjection volume: 20 µL of 10 µg/mL sampleDetection: UV @ 280 nm


2. Theophylline

Theophylline and Theobromine

1. Theobromine

N

N N

N

O

O CH2

H3C

CH3

3. Caffeine

Minutes


HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µmPart number: 186000108Mobile phase: 50 mM phosphate, pH7.0/methanol 36:64Flow rate: 1.0 mL/minInjection volume: 25 µLDetection: UV @ 250 nm


Trazodone

1. 1-(3-chlorophenyl)peperazine

3. Trazodone

2. Maprotiline (I.S.)

Minutes



Condition: 3 mL methanolRinse: 3 mL H2O


Wash:1 mL H2O

Elute:1.2 mL methanol

Evaporate to 0.2 mL

Reconstitute to exactly 1.0 mL with H2O


Compounds % RecoveryTap Water Tap WaterSpike Level Spike Level500 µg/L 200 ng/L5 replicates 7 replicates

1. Desisopropylatrazine 98.4 (5.0) 95.6 (5.8)2. Hydroxyatrazine 132 (1.3) 109 (11)3. Desethylatrazine 106 (5.1) 104 (4.0)4. Simazine not determined 97.7 (3.9)5. Cyanazine not determined 93.1 (3.7)6. Atrazine 101 (5.0) 101 (4.4)

Triazine Herbicides in Drinking Water

HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µmPart number: WAT0200655Mobile Phase A: 5 mM phosphate buffer, pH 6.7/Acetonitrile 85:15 Mobile Phase B: AcetonitrileGradient: Time Profile

(min) %A %B0 100 02 100 025 30 70


1

2

34

5 6

Minutes0 5 10 15

blank cartridge

spiked well water

nonspiked sample

6. Atrazine

3. Desethylatrazine2. Hydroxyatrazine

4. Simazine 5. Cyanazine

1. Desisopropylatrazine

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: 20 mM potassium phosphate, pH 7/methanol 35:65Flow rate: 1.0 mL/minInjection volume: 20 µL of 100 µg/mL sampleDetection: UV @ 254 nm

USP Tailing Factors1. 1.72. 1.73. 1.84. 1.55. 1.46. 1.2

Tricyclic Antidepressants

1. Protriptyline HCL

2. Nortriptyline HCL

3. Doxepin HCL

4. Imipramine HCL

5. Amtriptyline HCL

6. TrimipramineMinutes


HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart number: WAT046980Mobile phase: 20 mM potassium phosphate, pH 7.0/methanol 29:71Flow rate: 1.0 mL/minInjection volume: 5 µL of 1 to 1.16 mg/mLTemperature: 35˚ CDetection: UV @ 254 nm


1. Nordoxepin HCL

2. Doxepin HCL

4. Amtriptyline HCL

3. Nortriptyline HCL

Tricyclic Antidepressants and Metabolites

Minutes


Tricyclic Antidepressants in Plasma

500 ng/mL 100 ng/mL

Compound Recovery RSD Recovery RSD(n=96) (n=95)

Nortriptyline 92.3% 1.4% 90.8% 5.7%

Doxepin 90.6% 1.4% 90.4% 4.7%

Imipramine 92.2% 1.7% 86.4% 5.3%

Amitriptyline 90.2% 1.6% 85.3% 5.8%

Trimipramine 90.3% 1.9% 89.8% 6.1%

0 1 2 3 4

B

A

0.02 AU

1

2 34

56





Load1 mL spiked plasma plus

20 µL concentrated phosphoric acid

WashA. 1 mL 2% ammonium

hydroxide in 5% methanolB. 1 mL 2% ammonium

hydroxidein 65% methanolC. 1 mL 2% acetic acid in 5% methanol

Elute600 µL 65% methanol

Add internal standard (I.S.)60 µL 36 µg/mL nordoxepin in


HPLC Method

Column: SymmetryShield™ RP8, 4.6 x 75 mm, 3.5 µmPart number: WAT094263Mobile phase: 50 mM phosphate, pH 7/methanol 26:74Flow rate: 1.4 mL/minInjection volume: 1 mL spiked plasma plus 20 µL concentrated phosphoric acid, 100 µL injectionTemperature: 29˚ CDetection: UV @ 254 nm

Compounds:Spiked at 500 ng/mL versus Blank:1. Nordoxepin (I.S.)2. Nortriptyline3. Doxepin4. Imipramine5. Amitriptyline6. Trimipramine

3. Doxepin1. Nordoxepin 2. Nortriptyline

4. Imipramine 5. Amitriptyline 6. Trimipramine

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20 mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: 50 mM potassium phosphate, pH 3.0/acetonitrile 85:15Flow rate: 1.0 mL/minInjection volume: 10 µL of 200 µg/mL sampleDetection: UV @ 261 nm


Tripelennamine

1. Tripelennamine

Minutes


Verapamil

HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µm Guard Column: Sentry™ Guard Column 3.9 x 20mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250 Mobile phase: 10 mM sodium acetate with 3.3% glacial acetic acid, pH 2.6/acetonitrile 70:30Flow rate: 1.0 mL/minInjection volume: 10 µL of 100 µg/mL sampleDetection: UV @ 278 nm


1. Verapamil

Minutes


Verapamil and Norverapamil

HPLC Method

Column: SymmetryShield™ RP8, 3.9 x 150 mm, 5 µm Part number: WAT200655Mobile phase: 50 mM phosphate pH 7.0/acetonitrile/methanol 41:37:22Flow rate: 1.0 mL/minInjection volume: 40 µLDetection: UV @ 230 nm


1. Norverapamil

2. Verapamil

3. Methoxyverapamil (I.S.)

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µmGuard Column: Sentry™ Guard Column 3.9 x 20mm, 5 µmPart numbers: Column - WAT046970, Guard - WAT054250Mobile phase: Methanol/acetonitrile/water 45:45:10Flow rate: 1.0 mL/minInjection volume: 10 µL of 25 µg/mL sampleDetection: UV @ 280 nm

USP Tailing Factors1. 1.332. 1.203. 1.16 Vo. Uracil

1. Trans-Retinol (Vitamin A)

2. Cholecalciferol (Vitamin D3)

3. Alpha-Tocopherol (Vitamin E)

Vitamins- Fat-Soluble

Minutes


Vitamins- Water-Soluble

1. Niacinamide

6. Riboflavin

7. Thiamine Hydrochloride

2. Calcium Pantothenate

3. Pyridoxal

4. Pyrodoxine Hydrochloride

5. Pyridoxamine Dihydrochloride

HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart numbers: Column - WAT046980, PIC B6 - WAT084199Mobile phase: 20 mM PIC B6 (hexane sulfonic acid) and 0.1% phosphoric acid,

pH 2.2/methanol 75:25Flow rate: 0.7 mL/minInjection volume: 10 µL of mixture with component 1 at 11 µg/mL, 2 at 133 µg/mL,

3 at 17 µg/mL, 4 at 6 µg/mL, 5 at 25 µg/mL, 6 at 34 µg/mL, and 7 at 67 µg/mL

Detection: UV @ 210 nm

USP Tailing Factors1. n.c.2. n.c.3. 1.44. 1.15. 1.26. 1.17. 1.2

Minutes


HPLC Method

Column: Symmetry® C18, 3.9 x 150 mm, 5 µmPart numbers: Column - WAT046980, PIC B6 - WAT085140Mobile phase: 20 mM PIC B6 (hexane sulfonic acid) and 0.1% phosphoric acid, pH 2.2/methanol 75:25Flow rate: 0.7 mL/minInjection volume: 10 µL of mixture with 0.02 to 0.17 mg/mLTemperature: 40˚ CDetection: UV @ 280 nm


Vitamins- Water-Soluble Folic Acid Mixture

1. Nicergoline

2. Folic Acid

3. Riboflavin

4. Thiamine Hydrochloride

Minutes


HPLC Method

Column: Symmetry® C8, 3.9 x 150 mm, 5 µmPart number: WAT046970Mobile phase: 50 mM potassium phosphate, pH 4.6/methanol 85:15Flow rate: 1.0 mL/minInjection volume: 20 µL of 100 µg/mL sampleDetection: UV @ 254 nm


1. Zidovudine

Zidovudine (AZT)

Minutes


Particle Part No. Part No.Dimension Size C18 C81.0 x 50 mm 3.5 µm WAT106056 WAT1060521.0 x 150 mm 3.5 µm WAT248059 WAT2480722.1 x 30 mm 3.5 µm WAT058973 WAT0589772.1 x 50 mm 3.5 µm WAT200650 WAT2006242.1 x 100 mm 3.5 µm WAT058965 WAT0589612.1 x 150 mm 3.5 µm WAT106005 WAT1060113.0 x 100 mm 3.5 µm 186000696 1860006983.0 x 150 mm 3.5 µm 186000695 1860006974.6 x 30 mm 3.5 µm 186000271 1860002704.6 x 50 mm 3.5 µm WAT200625 WAT2006204.6 x 75 mm 3.5 µm WAT066224 WAT0662004.6 x 100 mm 3.5 µm WAT066220 WAT0662044.6 x 150 mm 3.5 µm WAT200632 WAT200630

2.1 x 50 mm 5 µm 186000206 1860002122.1 x 150 mm 5 µm WAT056975 WAT0569553.0 x 150 mm 5 µm WAT054200 WAT0542303.0 x 250 mm 5 µm 186000690 1860006913.9 x 150 mm 5 µm WAT046980 WAT0469704.6 x 50 mm 5 µm 186000207 1860002134.6 x 150 mm 5 µm WAT045905 WAT0459954.6 x 250 mm 5 µm WAT054275 WAT054270

Symmetry® Analytical Columns

Particle Part No. Part No.Dimension Size C18 C82.1 x 20 mm 3.5 µm 186000269 1860002682.1 x 50 mm 3.5 µm 186000152 1860001492.1 x 100 mm 3.5 µm 186000151 1860001532.1 x 150 mm 3.5 µm 186000150 1860001484.6 x 75 mm 3.5 µm WAT066260 WAT0662104.6 x 100 mm 3.5 µm WAT066265 WAT066215

3.9 x 50 mm 5 µm WAT054220 WAT0542403.9 x 150 mm 5 µm WAT054205 WAT0542354.6 x 150 mm 5 µm WAT054210 WAT0542554.6 x 250 mm 5 µm WAT054215 WAT054245

Symmetry® Cartridge Columns (Requires endfittings, see Page 186)

Particle Part No. Part No.Dimension Size C18 C82.1 x 10 mm 3.5 µm WAT106127 WAT1061283.9 x 20 mm 5 µm WAT054225 WAT054250

Symmetry® Sentry™ Guard Columns (2 per pack)(Requires Sentry™ Guard Holders, see Page 186)

Particle Part No. Part No.Dimension Size C18 C80.32 x 50 mm 3.5 µm 186000945 1860009460.32 x 100 mm 3.5 µm 186000951 1860009520.32 x 150 mm 3.5 µm 186000957 186000958

0.32 x 50 mm 5 µm 186000929 1860009300.32 x 100 mm 5 µm 186000935 1860009360.32 x 150 mm 5 µm 186000347 186000941

Symmetry® Capillary Columns

Symmetry® Columnsand Cartridges

Dimension Particle Size Part Number

75 µm x 50 mm 3.5 µm 18600140775 µm x 100 mm 3.5 µm 18600140875 µm x 100 mm 5 µm 18600140975 µm x 150 mm 5 µm 186001410

Symmetry® C18 PicoFrit™ Columns

Dimension Particle Size Part Number

75 µm x 50 mm 3.5µm 18600140375 µm x 100 mm 3.5 µm 18600140475 µm x 100 mm 5 µm 18600140575 µm x 150 mm 5µm 186001406

Symmetry® C18 IntegraFrit™ Columns

Particle Part No. Part No.Dimension Type Size C18 C84.6 x 150 mm Column 3.5 µm WAT094240 WAT0942372.1 x 150 mm Column 5 µm WAT094234 WAT0942313.0 x 150 mm Column 5 µm WAT054446 WAT0544343.9 x 150 mm Column 5 µm WAT047210 WAT0469554.6 x 150 mm Column 5 µm WAT054448 WAT0544354.6 x 250 mm Column 5 µm WAT054450 WAT054438

3.9 x 150 mm Cartridge* 5 µm WAT054452 WAT0544404.6 x 150 mm Cartridge* 5 µm WAT054454 WAT0544424.6 x 250 mm Cartridge* 5 µm WAT054456 WAT054444

* Require Endfittings, see Page 13

Symmetry® Column and Cartridge ColumnMethod Validation Kits Three Columns from Three Different Batches to Test Reproducibility.

Particle Part No. Part No.Dimension Size C18 C87.8 x 10 mm 5 µm 186000711 1860007127.8 x 50 mm 5 µm 186000208 1860002147.8 x 100 mm 5 µm 186000209 18600021519 x 10 mm 5 µm 186000715 18600071619 x 50 mm 5 µm 186000210 18600021619 x 100 mm 5 µm 186000211 18600022930 x 50 mm 5 µm 186000235 18600023730 x 100 mm 5 µm 186000236 186000238

7.8 x 10 mm 7 µm 186000713 1860007147.8 x 150 mm 7 µm WAT066288 WAT0662857.8 x 300 mm 7 µm WAT066235 WAT06622519 x 10 mm 7 µm 186000717 18600071819 x 150 mm 7 µm WAT066240 WAT06622819 x 300 mm 7 µm WAT066245 WAT066230

Purification and Isolation Cartridge Column Holders

7.8 x 10 mm 5, 7 µm — 18600070819 x 10 mm 5, 7 µm — 186000709

Replacement o-ring 7.8 mm, 2 pkg 700001019Replacement o-ring 19 mm, 2 pkg 700001020

SymmetryPrep™ Columns for Purification and Isolation


Particle Part No. Part No.Dimension Size RP18 RP80.32 x 50 mm 3.5 µm 186000947 1860009480.32 x 100 mm 3.5 µm 186000953 1860009540.32 x 150 mm 3.5 µm 186000959 186000960


SymmetryShield™ Capillary Columns

SymmetryShield™

Columns and Cartridges

Symmetry300™

Columns and Cartridges

Particle Part No. Part No.Dimension Size RP18 RP81.0 x 50 mm 3.5 µm 186000175 WAT1060601.0 x 150 mm 3.5 µm 186000176 WAT1060482.1 x 30 mm 3.5 µm 186000171 WAT1060012.1 x 50 mm 3.5 µm 186000172 WAT0942572.1 x 100 mm 3.5 µm 186000173 WAT0589692.1 x 150 mm 3.5 µm 186000174 WAT1060083.0 x 100 mm 3.5 µm 186000700 1860007033.0 x 150 mm 3.5 µm 186000699 1860007024.6 x 50 mm 3.5 µm 186000177 WAT0942604.6 x 75 mm 3.5 µm 186000178 WAT0942634.6 x 100 mm 3.5 µm 186000179 WAT0942664.6 x 150 mm 3.5 µm 186000180 WAT094269

2.1 x 50 mm 5 µm 186000217 1860002232.1 x 150 mm 5 µm 186000111 WAT0942453.0 x 150 mm 5 µm 186000692 WAT0942433.0 x 250 mm 5 µm 186000693 1860006943.9 x 150 mm 5 µm 186000108 WAT2006554.6 x 50 mm 5 µm 186000218 1860002244.6 x 150 mm 5 µm 186000109 WAT2006624.6 x 250 mm 5 µm 186000112 WAT200670

SymmetryShield™ Columns

Particle Part No. Part No.Dimension Size RP18 RP82.1 x 50 mm 3.5 µm 186000168 1860001472.1 x 100 mm 3.5 µm 186000167 1860001462.1 x 150 mm 3.5 µm 186000166 1860001454.6 x 75 mm 3.5 µm 186000183 WAT0942724.6 x 100 mm 3.5 µm 186000170 WAT094275

3.9 x 50 mm 5 µm — WAT0942483.9 x 150 mm 5 µm 186000106 WAT2006584.6 x 150 mm 5 µm 186000110 WAT2006654.6 x 250 mm 5 µm 186000113 WAT200661

SymmetryShield™ Cartridge Columns (Requires endfittings, see Page 186)

Particle Part No. Part No.Dimension Size RP18 RP82.1 x 10 mm 3.5 µm 186000169 WAT1061293.9 x 20 mm 3.5 µm 186000701 1860007043.9 x 20 mm 5 µm 186000107 WAT200675

SymmetryShield™ Sentry™ Guard Columns (2 per pack)(Requires Sentry™ Guard Holders, see Page 186)

Particle Part No. Part No.Dimension Size RP18 RP819 x 10 mm 5 µm 186001835 18600184119 x 50 mm 5 µm 186001836 18600184219 x 100 mm 5 µm 186001837 18600184319 x 150 mm 5 µm 186001838 186001844

19 x 150 mm 7 µm 186001839 18600184519 x 300 mm 7 µm 186001840 186001846


7.8 x 10 mm 5, 7 µm — 18600070819 x 10 mm 5, 7 µm — 186000709


SymmetryShield™ Columns for Purification and Isolation

Particle Part No. Part No.Dimension Size C18 C41.0 x 150 mm 3.5 µm 186000185 1860002762.1 x 50 mm 3.5 µm 186000187 1860002772.1 x 100 mm 3.5 µm 186000188 1860002782.1 x 150 mm 3.5 µm 186000200 1860002794.6 x 50 mm 3.5 µm 186000201 1860002804.6 x 75 mm 3.5 µm 186000189 1860002814.6 x 100 mm 3.5 µm 186000190 1860002824.6 x 150 mm 3.5 µm 186000197 186000283

2.1 x 150 mm 5 µm WAT106172 1860002853.9 x 150 mm 5 µm WAT106154 1860002864.6 x 50 mm 5 µm WAT106209 1860002874.6 x 150 mm 5 µm WAT106157 1860002884.6 x 250 mm 5 µm WAT106151 186000289

Symmetry300™ Analytical Columns

Particle Part No. Part No.Dimension Type Size RP18 RP82.1 x 150 mm Column 3.5 µm 186000182 —4.6 x 150 mm Column 3.5 µm 186000181 WAT0942782.1 x 150 mm Column 5 µm 186000100 WAT0942543.0 x 150 mm Column 5 µm - WAT0942513.9 x 150 mm Column 5 µm 186000104 WAT2105944.6 x 150 mm Column 5 µm 186000103 WAT2105884.6 x 250 mm Column 5 µm 186000102 WAT210591

3.9 x 150 mm Cartridge* 5 µm 186000105 WAT2105824.6 x 150 mm Cartridge* 5 µm 186000101 WAT2105854.6 x 250 mm Cartridge* 5 µm 186000114 WAT210579

* Require endfittings, see Page 186

SymmetryShield™ Column and Cartridge ColumnMethod Validation Kits Three Columns from Three Different Batches to Test Reproducibility.


Particle Part No.Dimension Size C1819 x 10 mm 5 µm 18600184719 x 50 mm 5 µm 18600184819 x 100 mm 5 µm 18600184919 x 150 mm 5 µm 186001850


7.8 x 10 mm 18600070819 x 10 mm 186000709


Symmetry300™ Columns for Purification and Isolation

Particle Part No.Dimension Size C182.1 x 50 mm 3.5 µm 1860001992.1 x 100 mm 3.5 µm 1860001912.1 x 150 mm 3.5 µm 1860001964.6 x 75 mm 3.5 µm 1860001924.6 x 100 mm 3.5 µm 186000193

3.9 x 150 mm 5 µm WAT1061694.6 x 150 mm 5 µm WAT1061634.6 x 250 mm 5 µm WAT106160

Symmetry300™ Cartridge Columns (Requires endfittings, see )

Particle Part No. Part No.Dimension Size C18 C42.1 x 10 mm 3.5 µm 186000198 1860002753.9 x 20 mm 5 µm WAT106166 186000284

Symmetry300™ Sentry™ Guard Columns (2 per pack)(Requires Sentry™ Guard Holders, see Page 186)

Particle Part No. Part No.Dimension Size C18 C40.32 x 50 mm 3.5 µm 186000949 1860009500.32 x 100 mm 3.5 µm 186000955 1860009560.32 x 150 mm 3.5 µm 186000961 186000962


Symmetry300™ Capillary Columns

Particle Part No. Part No.Dimension Type Size C18 C42.1 x 150 mm Column 3.5 µm 186000194 1860002904.6 x 150 mm Column 3.5 µm 186000195 186000291

2.1 x 150 mm Column 5 µm WAT106193 1860002923.9 x 150 mm Column 5 µm WAT106187 1860002934.6 x 150 mm Column 5 µm WAT106190 1860002944.6 x 250 mm Column 5 µm WAT106184 186000295

3.9 x 150 mm Cartridge* 5 µm WAT106181 —4.6 x 150 mm Cartridge* 5 µm WAT106175 —4.6 x 250 mm Cartridge* 5 µm WAT106178 —

* Require endfittings, see Page 186

Symmetry300™ Column and Cartridge ColumnMethod Validation Kits Three Columns from Three Different Batches to Test Reproducibility.

Particle Symmetry® Symmetry®

Dimension Size C18 C82.1 x 20 mm 3.5 µm 186002066 1860020672.1 x 20 mm 3.5 µm 186002070 1860020713.0 x 20 mm 3.5 µm 186002074 186002075

3.0 x 20 mm 5 µm 186002078 1860020793.9 x 20 mm 5 µm 186002082 1860020833.9 x 20 mm 5 µm 186002086 1860020874.6 x 20 mm 5 µm 186002090 1860020914.6 x 20 mm 5 µm 186002094 186002095

Symmetry IS™ Columns

Particle Symmetry® Symmetry®

Dimension Size RP18 RP82.1 x 20 mm 3.5 µm 186002068 1860020692.1 x 20 mm 3.5 µm 186002072 1860020733.0 x 20 mm 3.5 µm 186002076 186002077

3.0 x 20 mm 5 µm 186002080 1860020813.9 x 20 mm 5 µm 186002084 1860020853.9 x 20 mm 5 µm 186002088 1860020894.6 x 20 mm 5 µm 186002092 1860020934.6 x 20 mm 5 µm 186002096 186002097

SymmetryShield IS™ Columns

Particle Symmetry300™

Dimension Size C180.35 x 5 mm 5 µm 186001492

Opti-Pak™ Symmetry300™ C18 trap columns (5 per pack)


Cartridge and Guard Columns

Integrated Sentry™ Guard Holder to gowith cartridge end-fittings (see above)

3.0 x 20 mm, 3.9 x 20 mm – use Part Number WAT046905

Universal Sentry™ Guard Holder (Use on any column)

2.1 x 10 mm use Part Number WAT0979582.1 x 20 mm use Part Number 1860002623.0 x 20 mm use Part Number WAT0469103.9 x 20 mm use Part Number WAT0469104.6 x 20 mm use Part Number WAT046910

Waters Cartridge Column

Waters cartridge system requires re-useable endfittings. These cartridge endfit-tings need to be ordered when purchasing a Waters HPLC cartridge columnfor the first time. These cartridge columns should be connected to your HPLCinstrument using Waters standard connectors.

Disposable Cartridge

Reusable End Connectors

Waters Cartridge Column

ConnectorEndfitting

WAT037525

C-Clip

GrooveRetaining

Nut

Cartridge

Waters Sentry™ Guard Column andUniversal Guard Holder

Waters offers a line of Sentry™ Guard columns that contain the same high performance packing materials as all of the Waters analytical columns.Developed for customers needing increased capacity for biological fluid clean-up and/or temperature control, the Sentry™ Guard column is available in twoholder designs--one to be used as an integrated part of the Waters steel cartridge column with reusable endfitting, the other for use with any HPLC column. Both are installed without tools.

Sentry™ Guard Column

Integrated Guard Holder

Universal Guard Holder

Cartridge End-Fittings

2.1 x 50 mm, 2.1 x 100 mm, 2.1 x 150 mm, 2.1 x 250 mm use Part Number 7000001173.0 x 50 mm, 3.0 x 100 mm, 3.0 x 150 mm, 3.0 x 250 mm use Part Number WAT0375253.9 x 50 mm, 3.9 x 100 mm, 3.9 x 150 mm, 3.9 x 250 mm use Part Number WAT0375254.6 x 50 mm, 4.6 x 100 mm, 4.6 x 150 mm, 4.6 x 250 mm use Part Number WAT037525

Sentry™ Guard Column

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