Pharmaceutical Compounds Cosmetics

ON HPLC COLUMNS

AUTHORIZED DISTRIBUTOR MZ-Analysentechnik GmbH, Barcelona-Allee 17• D-55129 Mainz Tel +49 6131 880 96-0, Fax +49 6131 880 96-20 e-mail: [email protected], www.mz-at.de No.TI007E

Pharmaceutical compounds (1)

O A:H2O/TFA = 100/0.1 CH3 CH 150 3 CH3 B:ACN/TFA = 100/0.1 CH2CHC(CH2)3CH(CH2)3CH(CH2)3CH 75-100%B (0-2min) O CH CH CH3 3 3 1.0 mL/min phytomenadione UV at 220nm 100 Vitamin K1 37 deg.C mAU

COOH 150 O O N CH3 0 CNH S H H H NH2 0.0 0.5 1.0 1.5 2.0 cefalexin min 100 mAU

A:H2O/TFA = 100/0.1 50 B:ACN/TFA = 100/0.1 0-30%B (0-2min) 1.0 mL/min 0 UV at 220nm 37 deg.C 0.0 0.5 1.0 1.5 2.0 min

A:H2O/TFA = 100/0.1 O B:ACN/TFA = 100/0.1 150 NH N O O N 30-55%B (0-2min) N N H 1.0 mL/min O UV at 220nm 100 pranlukast 37 deg.C mAU

H3C N NH2 0 150 N CHO CH2N S SCH C C 2 O 0.0 0.5 1.0 1.5 2.0 H3C CH2CH2OH min fursultiamine 100 mAU

A:H2O/TFA = 100/0.1 B:ACN/TFA = 100/0.1 2-20%B (0-2min) 0 1.0 mL/min 0.0 0.5 1.0 1.5 2.0 UV at 220nm min 37 deg.C

TI007E-AB27 No.TI009E

LC-ESI-MS application

75 x 2 mm

1 nilvadipine

2 nisoldipine

1 2 3 4 5 6 min

Cadenza CD-C18, 75 x 2.0 mm 60% acetonitrile, 0.2 mL/min, 40 °C Negative-ESI

TI009E-ZJ06 No.TI012E

Metabolites of organic solvents

OH O 1 CH C OH N2 = 41200 30 mandelic acid 2

OH O Rs (5/4) = 1.88 2 CH NHCH2 C OH 20 hippuric acid 4 5

1 3 OH O 3 CH NHCH2 C OH mAU 10 CH3 o-methylhippuric acid

OH O 0 4 H3C CH NHCH2 C OH p-methylhippuric acid 0 5 10 15 20 25

min OH O 5 CH NHCH2 C OH

H3C m-methylhippuric acid

Cadenza CD-C18, 250 x 4.6 mm methanol / 20 mM KH2PO4 = 30 / 70 0.5 mL/min, 30 °C UV at 225 nm 16.2 MPa

TI012E-ZI27 No.TI013E

Estrogens

1 HO estrone O 2

HO 2 OCH3 4-hydroxyestrone 4-methyl ether 1 3 4 1 O 2 H3CO mAU 5 3 HO 2-hydroxyestrone 2-methyl ether

HO 0 5 10 15 20 25 min 4 H3CO 2-hydroxyestrone 3-methyl ether

H3CO 5 OH Cadenza CD-C18, 150 x 4.6 mm 4-hydroxyestrone 3-methyl ether ACN / water = 44 / 56 1.0 mL/min, 9.8 MPa, 37 °C UV at 280 nm 5 uL inj. (50 ng)

Courtesy of Prof. Dr. K. Shimada and Dr. K. Mitamura, Kanazawa Univ.

TI013E-ZK06 No.TI016E

Acetylsalicylic acid from Tablet

400 400 400

300 300 300

200 200 200 mAU mAU mAU

100 100 100

0 0 0

0 1 min 2 0 1 min 2 0 1 min 2 1.0 mL/min 0.5 mL/min 0.2 mL/min 5.0 MPa 4.3 MPa 4.2 MPa

Cadenza CD-C18 COOH ACN / water / acetic acid = 60 / 40 /0.1 OCCH UV at 260 nm, 37 °C 3 acetylsalicylic acid from tablet O 5 mg/mL, 0.4 uL Acetylsalicylic acid

TI016E-AA16 No.TI027E

Vitamin preparation

1 O C NH2

N 1 3 4 5 6 nicotinamide 60

2 H OH

O C O 2 HOCH2 HO OH 40 L-ascorbic acid

3 CH2OH mAU HO CH2OH 20 H3C N 7 pyridoxine

0 4 O CH3 H3C N N 0 5 10 15 N min O N CH3 caffeine

5 OH OH OH O CH2CH CH CHCH2 O P ONa

H3C N N O OH NH H3C N Cadenza CD-C18, 50 x 4.6 mm O A: 0.3%TFA B: methanol riboflavin monophosphate 0-40%B (0-7min) sodium salt 40-100%B (7-7.5min) 100%B (7.5-15min) 6 0.8 mL/min, 37 °C COOH UV at 280 nm, 3.4 MPa 7 benzoic acid O CH3 H3C C O CH3 O H3C CH2CH2CH2CH CH3 CH3 CH3 3 Vitamin E acetate

TI027E-AB16 No.TI029E

Squalene

H3C CH3 CH3 CH3 CH3 CH3

H3C CH3

200

mAU 100

0 0.0 2.5 5.0 7.5 10.0 12.5 15.0 min

Cadenza CD-C18, 75 x 4.6 mm methanol 1.0 mL/min, 37 °C 3.2 MPa UV at 210 nm

TI029E-AC15 No.TI050E

Lavender Oil

20 mAU

0 0 10 20 30 40 50 60 70 min 80

Cadenza CD-C18, 250 x 4.6 mm A: 0.1% formic acid in water B: 0.1% formic acid in ACN 10-100%B (0-70min), 100%B (70-80min) 1.0 mL/min UV at 254 nm

TI050E-AG14 No.TI054E

LC-MS/MS High Throughput Analysis

LC beta-estradiol 1 pg/uL, 10uL injection

[LC] Cadenza CD-C18, 50 x 2 mm methanol / water = 75 / 25 0.2 mL/min, 40 °C

[MS] API 4000 0 0.5 1.0 1.5 2.0 2.5 min ESI-negative

m/z 271 OH MS H3C

H H H

HO beta-estradiol

MS/MS

Courtesy of TAKARA SHUZO CO., LTD.

TI054E-AI19 No.TI063E

Steroid Hormones

O 1 H3C

CH3 H H H O androstene-3,17-dione 1 2 3 OH 4 2 H3C CH3 H H H O testosterone

CCH3 3 H3C OH CH3 H H H O 17 a -hydroxyprogesterone

CCH3 4 H3C CH3 H 7 H H O 6 progesterone 5

Cadenza CD-C18, 75 x 2 mm A: 10% methanol, B: methanol 30 - 50 %B (0 - 0.5 min), 50 - 80 %B (0.5 - 12.5 min),100 %B (12.5 min - ) 0.3 mL/min UV at 260 nm 20 µL ( 500 ppb )

TI063E-BB26

Courtesy of Pharma Foods International Co., Ltd. No.TI072E

Local Anesthetic and Angiotonic

1 HO 30 H OH CCH NHCH HCl 3 2 3 Phenylephrine 20 4

2 2 mAU 1 CH3 10 O CH2CH3 NH C OCH2N CH2CH3 CH3

0 Lidocaine

0 2 4 6 8 10 3 min N HCl N CH2

Naphazoline

Unison UK-Phenyl, 75 x 4.6mm A:20mM H PO B:MeOH 4 3 4, O 0-70%B (0-10min) CH3 CH3(CH2)3NH C OCH2CH2N 1.0 mL/min, 5.7 MPa, CH3 37 °C, 254 nm Tetracaine

Courtesy of Prof. Ph.D. M.Mishima, Daiichi College of Pharmaceutical Sciences.

TI072E-BF25 No.TI075E

Impurities separation for pharmaceutical compound

Brand-A

150 x 4.6 mm 20 mM Na2SO4 / acetonitrile / acetic acid = 45 / 55 / 1 1.0 mL/min, 40 °C, UV at 254 nm

Courtesy of Hiroshi Okumura

TI075E-BI11 No.TI077E

Allergy Medications

CH3O HOOC 350 1 CH3O CH CH CONH tranilast 300 N NH2 5 N 3 2 HCl 250 4 epinastine, HCl 1 200 2 N CH3 CH2CH2 N 3 C CH H 3 HOOC COOH mAU Cl C C 150 H H chlorpheniramine, malate

100

CH3 4 CHOCH2CH2 N HCl 50 CH3 diphenhydramine, HCl

Cl 0 0 2 4 6 8 10 CH N N CH2CH2OCH2CH2OH min 5 COOH OH CH2 OH Unison UK-C8, 75 x 4.6 mm A: 20mM HCOONH4 B: ACN COOH 20-80%B ( 0-10 min ) hydroxyzine, pamoic acid salt 1.0 mL/min, 37 °C, 6.2 MPa, 230 nm 0.6-2 uL ( 0.3-10 ug )

TI077E-BI11 No.TI078E

Allergy Medications

CH3O HOOC 350 1 CH3O CH CH CONH tranilast 300 N NH2 N 2 HCl 250 3 5 epinastine, HCl

4 CH 200 1 N 3 CH2CH2 N 3 C CH H 3 HOOC COOH mAU 2 150 Cl C C H H chlorpheniramine, malate

100

CH3 4 CHOCH2CH2 N HCl 50 CH3 diphenhydramine, HCl

0 Cl

0 2 4 6 8 10 CH N N CH2CH2OCH2CH2OH min 5 COOH OH CH2 OH Unison UK-Phenyl, 75 x 4.6 mm A: 20mM HCOONH4 B: ACN COOH 20-80%B ( 0-10 min ) hydroxyzine, pamoic acid salt 1.0 mL/min, 37 °C, 5.9 MPa, 230 nm 0.6-2 uL ( 0.3-10 ug )

TI078E-BI12 No.TI079E

Allergy Medications

CH3O HOOC 350 1 CH3O CH CH CONH tranilast 300 N NH2 N 2 HCl 250 epinastine, HCl 1 3 4

200 N CH3 5 CH2CH2 N 3 C CH H 3 HOOC COOH mAU 2 Cl C C 150 H H chlorpheniramine, malate

100

CH3 4 CHOCH2CH2 N HCl 50 CH3 diphenhydramine, HCl

Cl 0 0 2 4 6 8 10 CH N N CH2CH2OCH2CH2OH min 5 COOH OH CH2 OH Unison UK-C18, 75 x 4.6 mm A: 20mM HCOONH4 B: ACN COOH 20-80%B ( 0-10 min ) hydroxyzine, pamoic acid salt 1.0 mL/min, 37 °C, 6.5 MPa, 230 nm 0.6-2 uL ( 0.3-10 ug )

TI079E-BI12 No.TI080E

Allergy Medications

CH3O HOOC 350 1 CH3O CH CH CONH tranilast 300 N NH2 N 2 HCl 250 epinastine, HCl 4 200 3 N CH3 CH2CH2 N 3 C CH H 3 mAU 1 2 5 HOOC COOH 150 Cl C C H H chlorpheniramine, malate 100

CH3 CHOCH2CH2 N HCl 50 4 CH3 diphenhydramine, HCl

0 Cl

0 2 4 6 8 10 CH N N CH2CH2OCH2CH2OH min 5 COOH OH CH2 OH Unison US-C18, 150 x 4.6 mm A: 20mM HCOONH4 B: ACN COOH 20-80%B ( 0-10 min ) hydroxyzine, pamoic acid salt 1.0 mL/min, 37 °C, 5.8 MPa, 230 nm 0.6-2 uL ( 0.3-10 ug )

TI080E-BI12 No.TI085E

High Throughput LC-MS Application for Local Anesthetic and Antiarrhythmic Drugs

OH CH3 OCH2CHCH2NHCH CH3 1 atenolol

Int. CH2 C NH2 Shimadzu LCMS-2010A O 160e3 O ( ESI, positive, SIM ) 10 CH2CH3 C OCH2CH2N 150e3 1 CH2CH3 140e3 3 2 procaine 130e3 4 2 NH2 120e3 OH 6 8 CH3 7 OCH2CHCH2NHCH 110e3 5 CH3 pindolol 100e3 3 N H 90e3 CH3 OCH2CHCH2NHCH 80e3 9 CH3 OH 70e3 4 metoprolol 60e3 CH2CH2OCH3 50e3 OH CH3 OCH2CHCH2NHCH 40e3 CH3

30e3 5 propranolol

20e3 OH CH3 OCH2CHCH2NHCH 10e3 CH3 6 CH2CH CH2 alprenolol 1.00 1.25 1.50 1.75 min

O CH3 C OCH2CH2N CH3 7 tetracaine

NH(CH2)3CH3

CH3 O CH2CH3 NH C CH2N Cadenza CD-C18, 30 x 2 mm 8 CH2CH3 lidocaine A: 10mM ammonium acetate CH3 O B: acetonitrile CH2CH3 C NHCH2CH2N 0 - 90 %B (0 - 1 min), 90 %B (1 - 2 min) CH2CH3 0.5 mL/min, 40 °C 9 dibucaine 10 pg/uL, 5uL N O(CH2)3CH3

CH3 10 NH C N bupivacaine O CH3 CH2(CH2)2CH3

TI085E-BJ02 No.TI089E

Column size comparison for elution of investigational medication

0.2 mL/min 500 µL inj.

0.4 mL/min 500 µL inj.

Brand-A 150 x 6 mm

1 mL/min 500 µL inj.

acetonitrile / water / phosphoric acid = 600 / 400 / 1, 40 °C, 280 nm

Courtesy of Hiroshi Okumura

TI089E-CF03 No.TI093E

LC-MS Application for Bug Repellent Active Ingredient

API3000 (TAKARA BIO INC. ) 1153 1100 H3C 100 fg 1000 H3C N 900 CH3

800 O

700 DEET (N,N-diethyl-m-toluamide) Mw. 191 600

500

400

300

200

100

0 0.5 1.0 1.5 2.0 2.5 3.0 min

Cadenza CD-C18, 50 x 2 mm 0.1% formic acid / 60% methanol, 0.2 mL/min, 40 °C, 5µL (20fg/µL) API3000: ESI, MRM Positive Q1/Q3: 192/119

Courtesy of J.Watanabe, TAKARA BIO INC.

TI093E-CF04 No.TI128E

PQQ ( pyrroloquinoline quinone )

mAU

200

Unison UK-C18 7.8 MPa

100 Unison UK-C8 6.8 MPa

Unison UK-Phenyl 0 6.8 MPa

0 2 4 6 8 10 min

O O O C OH N N H Unison, 75 x 4.6 mm 10mM DBA-Acetate / ACN = 85 / 15 HO C C OH 1.0 mL/min, 37 °C, UV at 260 nm O O PQQ 1 µg ( 2µL )

TI128E-CF11 No.TI132E

Urea

mAU 40 O H2N C NH2 urea

0 2 4 6 8 10 min

Unison UK-C18, 250 x 4.6 mm water / HFBA = 100 / 0.1 0.8 mL/min, ambient UV at 210 nm, 13 MPa 100 µg ( 20 µL )

TI132E-CF18 No.TI141E

Ascorbic Acid Derivative

1 2 H CH2OH 3 H OH CH2OH C O

C O O O HO OH C NH2 HOCH2 OH O HO OH HO O N OH O L-ascorbic acid L-ascorbic acid 2-glucoside nicotinamide

mAU 1 2

3 Unison UK-C18 75 x 3 mm 0.43 mL/min 200 6 MPa, 0.2 µL

100 Unison UK-C18 3 75 x 4.6 mm 1 mL/min 8 MPa, 0.4 µL

1 2 Unison US-C18 3 150 x 4.6 mm 1 mL/min 7 MPa, 0.4 µL 0

0 5 10 15 min

20mM ammonium acetate + 10mM dibutylammonium acetate 37 °C, 260 nm, 0.5 - 1.5 µg/µL

TI141E-CL17 No.TI154E

Ascorbic Acid Related Compounds

1 2 3 H CH2OH H OH H OH CH2OH C C O C O O HO OH HOCH2 O HOCH2 O OH O HO OH HO OH HO O OH O isoascorbic acid L-ascorbic acid L-ascorbic acid 2-glucoside

mAU

100

3 2 50

0 5 10 15 20 min

Unison UK-Silica, 150 x 4.6mm 50mM ammonium acetate / acetonitrile = 10 / 90 0.8mL/min, 30 °C, 260 nm, 2 µg

TI154E-DD08 No.TI155E

Ascorbic Acid Related Compounds

1 2 3 H CH2OH H OH H OH CH2OH C C O C O O HO OH HOCH2 O HOCH2 O OH O HO OH HO OH HO O OH O L-ascorbic acid isoascorbic acid L-ascorbic acid 2-glucoside

mAU Rs = 2.54 1 2

Unison UK-C18 75 x 4.6 mm 6 MPa 200

Rs = 2.53 1 2 100

Unison US-C18 150 x 4.6 mm 5 MPa 0

0 5 10 15 20 min

10mM dibutylammonium acetate 0.8mL/min, 30 °C, 260 nm, 2 µg

TI155E-DD08 No.TI156E

Thiamine HCl (Vitamin B1) Injection Solution

mAU NH2 CH2 N N+ CH3 CH CH OH H3C N S 2 2 thiamine

200

Unison UK-Phenyl Unison UK-C8 Unison UK-C18 Cadenza CL-C18 0

0 2 4 6 8 min

75 x 4.6 mm 50 mM HCOONH4 / acetonitrile= 98 / 2 1 mL/min, 37 °C, 260 nm, 0.2µL

TI156E-DD19 No.TI157E

Pyridoxine HCl (Vitamin B6) Injection Solution

CH2OH HO CH2OH

H3C N mAU pyridoxine 500

250

Unison UK-C18 Unison UK-Phenyl Unison UK-C8 Cadenza CL-C18 0

0 2 4 6 8 min

75 x 4.6 mm 50 mM HCOONH4 1 mL/min, 37 °C 260 nm, 0.5µL

TI157E-DD20 No.TI160E

Riboflavin Tetrabutyrate Tablet

mAU

OCOC3H7 OCOC3H7 CH2CH CH CHCH2OCOC3H7 OCOC3H7 H C N N O 200 3 NH H3C N O riboflavin tetrabutyrate

100

Unison UK-Phenyl, UKP03 Unison UK-C8, UK803 Cadenza CL-C18, CL003 Unison UK-C18, UK003

0 Cadenza CD-C18, CD003

0 2 4 6 8 10 min

75 x 4.6 mm 1% acetic acid / acetonitrile = 40 / 60 1 mL/min, 37 °C, 260 nm, 1 µg

TI160E-DE07 No.TI162E

Tocopherol Nicotinate Capsule

O CH3 C O CH3 O N H3C CH2CH2CH2CH CH3 CH3 CH3 3 mAU

100

Unison UK-Silica, 150 x 3 mm 0 hexane / THF = 95 / 5 0.5 mL/min (4MPa), 37 °C, 295 nm 0 5 10 15 min tocopherol nicotinate 5µg mAU

200

100

Cadenza CD-C18, 150 x 3 mm 0 methanol, 0.5 mL/min (6MPa) 37 °C, 295 nm 0 5 10 15 min tocopherol nicotinate 5µg

TI162E-DE24 No.TI165E

Antipyretic Analgesics

1 2 O 3 4 CH3 CH3 H3C N OH CH3 H N CH2CHN HOOC COOH CH3 HO N CCH3 CNH2 N N CH OH O O N O HO 2 2 CH3 S acetaminophen caffeine salicylamide promethazine methylenedisalicylate

mAU 1 2 3

400

200

0 2 4 6 8 10 min

Unison UK-C18, 75 x 3 mm A: water / trifluoroaceteic acid = 100/0.1 B: acetonitrile 10-60%B ( 0-6min ), 0.5 mL/min 37 °C, 260 nm, 0.6uL ( 6.5-0.3µg )

TI165E-DE28 No.TI173E

Acetylsalicylic Acid, Salicylic Acid

COOH mAU OCCH3 O acetylsalicylic acid 600

400

COOH OH salicylic acid 200

0 0 2 4 6 8 10 min

Cadenza CD-C18, 150 x 4.6 mm water / acetonitrile / formic acid = 60 / 40 / 0.1 0.6 mL/min (7MPa), room temp. 260 nm, 0.4µL (20µg)

TI173E-DF14 No.TI175E

Vitamin B12 Related Conpounds

mAU

200 NH2COCH2CH2 CH3 CH3 CH2CONH2 NH2COCH2 CH2CH2CONH2 H3C R cyanocobalamin N N H3C Co+ N CH3 N N CH3 NH2COCH2 N CH3 CH3 H3C CH3 CH2CH2CONH2 -HO H H O H O CH2CH2CONHCH2 C O P O H CH2OH H H3C O

R = -CN cyanocobalamin = -OH hydroxocobalamin

100 benzylalchol hydroxocobalamin

Unison UK-C18, 75 x 4.6 mm A: water / formic acid = 100 / 0.1 0 B: acetonitrile / formic acid = 100 / 0.1 0%B(0-3min), 0-30%B(3-8min) 0 5 10 min 1 mL/min (6MPa), 37 °C, 260 nm

TI175E-DG08 No.TI176E

Uracil, 5-Fluorouracil

mAU O O F HN HN

O N O N H H

400 uracil 5-fluorouracil

200 uracil 5-fluorouracil 0

0 2 4 6 8min

150 x 3 mm, 20 mM ammonium acetate 0.5 mL/min, 37 °C, 260 nm, 0.4 µg (0.4 µL)

TI176E-DG08

Courtesy of Dr. Naoki Komatsu, Kyoto Univ. No.TI181E

Xanthine Oxidase Related Compounds キサンチンオキシダーゼ関連化合物

1 O H N 2 HN O O N N H H 3 uric acid mAU 50 2 O HN N

N N 1 4 H hypoxanthine

3 O HN N

O N N H H xanthine

4 OH 6 min 0 2 4 N N N N H allopurinol

Unison UK-C18, 75 x 4.6 mm 50 mM NH4H2PO4, 1 mL/min (10MPa) 37 °C, 260 nm, 2 µL (0.2 µg)

TI181E-DG22 No.TI182E

Antifungal Drugs 抗真菌薬

1 1 N 2 N ·HNO3

mAU CH2 Cl CHOCH2 Cl Cl econazole nitrate

200 2 N

N ·HNO3 CH Cadenza CD-C18 2 Cl CHOCH2 Cl

Cl Cl miconazole nitrate

100 Cadenza CL-C18

Unison UK-C18

0 1 2 3 4 min

75 x 4.6 mm, water / acetonitrile / TFA =40 / 60 / 0.1 1 mL/min (7MPa), 37 °C, 230 nm, 0.4 µL (0.4 µg)

TI182E-DH03 No.TI194E

Hinokitiol

mAU O OH

100 CH hinokitiol H3C CH3

50 benzene

0 2 4 6 8 10min

Cadenza CD-C18, 75 x 4.6 mm 50mM ammonium acetate / acetonitrile = 60 / 40 1 mL/min (6MPa), 37 deg.C, 260 nm

TI194E-DI22 No.TI195E

Coenzyme Q10

mAU O CH3 H3CO H 10 400 H3CO CH3 O

200

Unison UK-Silica 150 x 3 mm

0 hexane / IPA = 998 / 2 0.5 mL/min, 37 deg.C 0 2 4 6 8 10 min 270 nm, 2ug (2uL)

mAU 1000

water / acetonitrile = 2 / 98

500 acetonitrile / tetrahydrofuran = 75 / 25

acetonitrile / tetrahydrofuran = 75 / 25

acetonitrile / tetrahydrofuran 75 x 3 mm = 75 / 25 0 0.5 mL/min, 37 deg.C 0 2 4 6 8 10min 270 nm, 2ug (2uL)

TI195E-DI27 No.TI197E

Antiseptics

mAU

CH3 CH3 CH3 + H3C C CH2 C (OCH2CH2)2 N CH2 - CH3 CH3 CH3 Cl

200

benzethonium chloride 10mg/mL x 2uL

100 CH3 + CH2 N R Cl- CH3

benzalkonium chloride 10% solution x 1uL 0

0 2 4 6 8 10 min

Unison UK-C8, 100 x 4.6 mm water / methanol / ammonium thiocyanate = 25 / 75 / 0.5 1.0 mL/min (9MPa), 37 deg.C, 260 nm

TI197E-DJ25 No.TI196E

Digitalis Glycosides

1 O 1 O mAU OH 100 CH3 H

CH3 H H OH HO H H 2 digoxigenin

O 2 O OH CH3 H

CH CH3 3 H O H OH 3 H O O H H HO 3 digoxin

3 O O

CH3 H

CH3 H H OH HO H H 4 digitoxigenin O 4 O

CH3 H

CH CH3 3 H O H OH H O O H H HO 3 digitoxin

0 5 10 min

Unison UK-C18, 75 x 4.6 mm water / acetonitrile = 60 / 40 1.0 mL/min (7MPa), 37 deg.C, 220 nm, 2 uL (0.2-0.8 ug)

TI196E-DJ27 No.TI201E

Non-Steroidal Anti-Inflammatory Drugs

O CH2CH2CH2CH3 N 1 N O

1 OH 2 5 oxyphenbutazone 3

mAU O 20 2 C CH3 CH C OH O 4 ketoprofen

6 O CH2CH2CH2CH3 3 N N O phenylbutazone

CH3 4 CH C OH O CH3O naproxen 0 5 10 15 20 min O C OH 5 N N H flunixin Cadenza CD-C18, 150 x 2 mm H3C CF3 water / methanol / formic acid (30 / 70 / 0.1) 0.2 mL/min (10MPa), 37 deg.C O 260 nm, 50 uL (12.5-100 ng) C ONa Cl CH3

6 NH

Cl meclofenamic acid sodium salt

TI201E-DK26 No.TI205E

LC-MS Application for Antiseptic Substance

Cl H H H NH NH N N N N N N NH NH H H H chlorhexidine Cl Mw 505.48 API4000 (TAKARA BIO INC. ) 1.41 Max. 1131.6 cps. 100% 95% 90% 85% 80% 75% 70% 2.5 pg 65% 60% 55% 50% 45% 40% 35% 30% 25% 20% 15% 10% 5% 0% 0.4 0.8 1.2 1.6 2.0 2.4 2.8 Time, min

Chlorhexidine Results.rdb (CH): "Linear" Regression ("1 / x" weighting): y = 1.43e+004 x + -15.5 (r = 0.9999)

1.4e5 1.4e5

1.3e5

1.2e5

1.1e5 1.0e5 r = 0.9999 9.0e4

8.0e4

7.0e4

6.0e4

5.0e4

4.0e4

3.0e4

2.0e4

1.0e4

0.0 0 1 2 3 4 5 6 7 8 9 10 Concentration, ng/mL

Unison UK-C8, 50 x 2 mm 0.1% formic acid / acetonitrile = 2 / 1, 0.2 mL/min, 5uL(500 fg/uL) API4000: ESI, MRM Positive, Q1/Q3 : 505 / 336

Courtesy of J.Watanabe, TAKARA BIO INC.

TI205E-DK30 No.TI206E

LC-MS Application for Calcium Antagonist

API4000 (TAKARA BIO INC. )

Max. 624.6 cps. 1.35 600 CH3 H O 500 S O 25 fg O 400 H HCl N CH O 3 300 N CH3 200 CH3 diltiazem HCl 100 Mw. 451

0 0.51.01.52.02.5 Time, min

Results.rdb (Diltiazem): "Linear" Regression ("1 / x" weighting): y = 5.98e+005 x + -22.1 (r = 0.9999)

3.0e6

2.8e6

2.6e6

2.4e6

2.2e6 2.0e6 r = 0.9999 1.8e6

1.6e6

1.4e6

1.2e6

1.0e6

8.0e5

6.0e5

4.0e5

2.0e5

0.0 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 Concentration, ng/mL

Unison UK-C8, 50 x 2 mm 0.1% formic acid / acetonitrile = 2 / 1, 0.25 mL/min, 5 uL(5 fg/uL) API4000: ESI, MRM Positive, Q1/Q3 : 415 / 178

Courtesy of J.Watanabe, TAKARA BIO INC.

TI206E-DK30

No.TI207E

LC-MS Application for Coenzyme Q10

API4000 (TAKARA BIO INC. )

2.04 Max. 131.6 cps. 132 O CH3 120 MeO H 10 100 500 fg MeO CH3 80 O Coenzyme Q10 60 Mw. 863.36

0 0.51.01.52.02.53.03.5 Time, min

CoenzymeQ10 Result.rdb (CoenzymeQ10): "Linear" Regression ("1 / x" weighting): y = 6.66e+003 x + 17.3 (r = 0.9998)

1.3e6

1.2e6

1.1e6

1.0e6 9.0e5 r = 0.9998 8.0e5

7.0e5

6.0e5

5.0e5

4.0e5

3.0e5

2.0e5

1.0e5

0.0 0 20 40 60 80 100 120 140 160 180 200 Concentration, ng/mL

Unison UK-C8, 75 x 3 mm 0.1% formic acid / acetonitrile / isopropanol = 1 / 5 / 5 0.8 mL/min, 10 uL(50 fg/uL) API4000: APCI, MRM Positive, Q1/Q3 : 863.5 / 197

Courtesy of J.Watanabe, TAKARA BIO INC.

TI207E-DL01 No.TI213E

Veterinary Medicine (Synthetic Antimicrobial)

HO O S CH3 O HO NH O Cl Cl thiamphenicol mAU 8

Unison UK-Phenyl

Unison UK-C8

Unison UK-C18 0

0 2 4 6 min

75 x 3 mm, 20mM HCOONH4 / acetonitrile = 88 / 12 0.5 mL/min (7MPa), 37 deg.C, 224 nm, 1ppm (5uL)

TI213E-DL21 No.TI214E

Veterinary Medicine (Antibiotic)

CH2CH2CH3 CH3 CH3 N HO C H mAU 100 C NH C H O HO O OH SCH3 OH lincomycin

Unison UK-Phenyl

Unison UK-C8

Unison UK-C18 0

0 2 4 6 8 min

75 x 3 mm, water / acetonitrile / trifluoroacetic acid = 90 / 10 / 0.1 0.5 mL/min (7MPa), 37 deg.C, 210 nm, 500ng / uL (5uL)

TI214E-DL21 No.TI215E

Veterinary Medicine (Antibiotic)

COOH H N O 2 O N CH3 CH3 C CNH S H H H ampicillin mAU 10

Unison UK-Phenyl Unison UK-C8 Cadenza CD-C18 Unison UK-C18 Cadenza CL-C18 0

0 2 4 6min

75 x 3 mm, water / acetonitrile / trifluoroacetic acid = 85 / 15 / 0.1 0.5 mL/min (7MPa), 37 deg.C, 210 nm, 10 ppm (2uL)

TI215E-DL21 No.TI216E

Veterinary Medicine (Antibiotic)

O OH O HO O OH C NH2

OH H HO CH3 CH3 OH N CH3 oxytetracycline mAU

Unison UK-Phenyl Unison UK-C8 Cadenza CD-C18 Cadenza CL-C18 Unison UK-C18 0 0 2 4 6 min

75 x 3 mm, water / acetonitrile / trifluoroacetic acid = 85 / 15 / 0.1 0.5 mL/min (7MPa), 37 deg.C, 270 nm, 1 ppm (10uL)

TI216E-DL22 No.TI219E

Veterinary Medicine (Antibiotic)

O CH3 H3C CH3 O OH H HO CH3 OH CH3 N H3C H3C OH O O CH3 CH3 H3C OH O H O CH O CH3 3 O CH3 erythromycin mAU 10

Unison UK-Phenyl

Unison UK-C8

Cadenza CD-C18

Unison UK-C18

Cadenza CL-C18 0

0 2 4 6 min

75 x 3 mm, 20mM HCOONH4 / acetonitrile = 70 / 30 0.5 mL/min (7-8MPa), 37 deg.C, 210 nm, 1 ug/uL (5uL)

TI219E-DL22 No.TI220E

Veterinary Medicine (Antibiotic)

H3C CH3 N CH3 O H O CH3 O HC H3C

CH3 HO N CH3 O O O H OH O H O CH3 H3C O O CH3 O OH R H3C spiramycin mAU

Unison UK-Phenyl

Unison UK-C8

Cadenza CD-C18

Cadenza CL-C18

Unison UK-C18 0

0 2 4 6 min

75 x 3 mm, water / acetonitrile / trifluoroacetic acid = 50 / 50 / 0.1 0.5 mL/min (6MPa), 37 deg.C, 230 nm, 1 ppm (5uL)

TI220E-DL22 No.TI221E

Veterinary Medicine (Antibiotic)

NH2 HO CH3 O H O N A: R = CH N NH 3 H H CH3 B: R = H H2N H2N OO H N H3C OH 2 CH3 O O O O H H H NH N N N CH R N H N N 3 H H H CH3 O O O CH3 H2N H2N colistin mAU

100 Unison UK-Phenyl

Unison UK-C8

Cadenza CD-C18

Unison UK-C18

Cadenza CL-C18

0 0 2 4 6 min

75 x 3 mm, A: water / trifluoroacetic acid = 100 / 0.1 B: acetonitrile / trifluoroacetic acid = 100 / 0.1 25-40 %B (0-5 min), 0.5 mL/min, 37 deg.C, 220 nm, 1 ug/uL (20uL)

TI221E-DL22 No.TI222E

Veterinary Medicine (Antibiotic)

CH3 NH2 H3C O O H HO O N HN H HN O S CH3 O H H O H CH O N N N N 3 HN N NH H O H O NH2 N H3C H3C O CH3 CH3 O NH O O NH HO HN O

NH2 bacitracin

Unison UK-Phenyl mAU Unison UK-C8 400

Cadenza CD-C18

Unison UK-C18

Cadenza CL-C18 0 0 2 4 6 min

75 x 3 mm, A: water / trifluoroacetic acid = 100 / 0.1 B: acetonitrile / trifluoroacetic acid = 100 / 0.1 10-40 %B (0-7 min), 0.5 mL/min, 37 deg.C, 220 nm, 1 ug/uL (2uL)

TI222E-DL24 No.TI224E

Natural Medicine Properties (Shoseiryuto)

1 CH2OH OO O 1 OH HO OH CH O O 2 OH C O

paeoniflorin

Cadenza CD-C18, 75 x 4.6 mm water / acetonitrile / H3PO4 = 700 / 100 / 1 1 mL/min, 25 deg.C, 230 nm

2 H CH3 HO C C NHCH3 H

- pseudoephedrine

3 H CH3 HO C C NHCH3 H

3 - ephedrine 2 Cadenza CD-C18, 75 x 4.6 mm water / acetonitrile / H3PO4 / SDS = 650 / 350 / 2 / 5 1 mL/min, 40 deg.C, 210 nm

TI224E-EB03 No.TI227E

ELSD application - taurine and water-soluble vitamins

NH2 O CH2 N N+ CH3 H2N CH2 CH2 S OH CH CH OH O H3C N S 2 2 1 taurine 2 thiamine (B1) V m 1 200 CH2OH HO CH2OH

H3C N 3 pyridoxine (B6) 100 2 7 5 6

3 4 O

C NH2 0 1 2 3 4 min 5 N 4 nicotinamide (B3) Unison UK-C18, 75 x 4.6 mm A: 5mM HCOONH4 B: methanol

10-50%B (0-2min), 50%B (2-5min) NH2COCH2CH2 CH3 CH3 CH2CONH2 1 mL/min, 10uL(500ng), ELSD(SofTA) NH2COCH2 CH2CH2CONH2 H C CN 3 N N H3C Co+ N CH3 N N CH3 NH2COCH2 N CH3 OH OH OH CH3 H3C CH2CH CH CHCH2OH O CH3 CH2CH2CONH2 CH3 H3C N H C N N -HO H 3 O N H O H O N CH2CH2CONHCH2 C O P O H NH O N CH2OH H3C N H O CH3 H3C O

7 riboflavin (B2) 6 caffeine 5 cyanocobalamin (B12)

Courtesy of Mr. Y.Sakai, M&S Instruments Trading Inc., Japan

TI227E-HF30 No.TI249E

Ingredients of Eydrops (allantoin and chlorpheniramine maleate)

1 H O N H2N O O N N H H mAU

1000 allantoin

1 2

N CH3 4uL ( 8, 0.08 ug ) CH2CH2 N C CH H HOOC 3 COOH C C Cl H H

chlorpheniramine, maleate

2uL ( 4, 0.04 ug )

1uL ( 2, 0.02 ug ) 0

0 5 10 min

Unison UK-Silica, 250 x 4.6 mm A: acetonitrile / acetic acid = 100 / 0.1 B: water / acetic acid = 100 / 0.1 0 - 40%B (0-10min) 1 mL/min , 37 deg.C, 220 nm

TI249E-EH18 No.TI256E

Nonsteroidal Antiinflammatory Drugs (NSAIDs)

1 O CH2CH2CH2CH3 3 N N O

1 OH oxyphenbutazone 2 2 O C CH3 4 CH C OH O 5 6 ketoprofen

mAU 3 400 CH3 1 2 3 CH C OH 4 O CH3O 5 naproxen 6 4 O CH2CH2CH2CH3 N 200 N O 1 2 3 4 phenylbutazone 5 5 6 O C OH

0 N N H 0 2 4 6 8 min H3C CF3 flunixin

6 O 75 x 4.6 mm C ONa Cl CH3 water / MeOH / HCOOH = 30 / 70 / 0.1 NH 1 mL/min, 37 deg.C, 240 nm, 2 uL(0.5ug) Cl meclofenamic acid sodium salt

TI256E-EI18 No.TI258E

Sulfonamides

O 7 1 N 5 NH S NH2 2 6 N O 3 sulfadiazine 4 8 O 2 N NH S NH2 1 S O sulfathiazole

mAU O 3 N NH S NH2 N O H3C sulfamerazine 100 H3C O 4 N NH S NH2 N O H3C sulfamethazine (sulfadimidin) H3CO 5 O N NH S NH2 N O sulfamonomethoxine 6 H3C O N O NH S NH2 O sulfamethoxazole 7 0 H3C N O O H3C 0 1.0 2.0 min NH S NH2 O sulfisoxazole 30 x 2 mm 8 N A: water / acetic acid = 100 / 0.1 O B: acetonitrile / acetic acid = 100 / 0.1 N NH S NH2 8%B (0-0.05min), 8-40%B (0.05-1.5min) O 0.8 mL/min, 37 deg.C, 280 nm, 1uL (20-50ng) sulfaquinoxaline

TI258E-EL20 No.TI259E

Sulfonamides O 1 H2N S NH2 sulfanilamide 1 O O O 2 H3C C NH S NH2 O sulfacetamide O 5 N 3 NH S NH2 N O sulfadiazine O 2 N 4 NH S NH2 6 8 S O sulfathiazole 12 7 O 4 10 5 N NH S NH2 9 14 11 O sulfapyridine mAU 3 13 16 O 15 N 6 NH S NH2 N O 100 H3C sulfamerazine H3C O N 7 NH S NH2 N O 1 H3C sulfamethazine 2 (sulfadimidin) 5 O 8 12 8 H3CO NH S NH2 6 N N 7 O 4 10 sulfamethoxypyridazine 9 14 O 11 13 16 3 15 9 Cl NH S NH2 N N O sulfachloropyridazine H3C O N sulfamethoxazole 10 O NH S NH2 O H3CO 1 5 O 2 11 N NH S NH2 N O 8 12 sulfamonomethoxine 6 7 H3C N 4 O 10 O 911 14 12 H3C 13 16 NH S NH2 3 15 O sulfisoxazole O O 13 C NH S NH2 O H3CO sulfabenzamide 0 O 14 N NH S NH2 0 5 10 15 min N O H3CO sulfadimethoxine N 75 x 4.6 mm O A: water / acetic acid = 100 / 0.1 15 N NH S NH2 B: methanol / acetic acid = 100 / 0.1 O sulfaquinoxaline 15-60 %B (0-18min), 1 mL/min (9MPa) 16 O O H3C C NH S NH NO2 37 deg.C, 260 nm, 2uL (40-120ng) O sulfanitran Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI259E-JB01 North America Other Countries No.TI264E

Parasympatholytics

1 H H O H O C C

O H3C N CH2OH H HBr H H scoporamine hydrobromide

2 H H O H O C C

H3C N CH2OH H 1/2 H SO mAU 2 4 3 H H 10 1 2 atropine sulfate 3 H H O H O C C + O CH3(CH2)3N CH3 CH2OH H Br- H H butylscopolamine bromide

75 x 4.6 mm 100mM ammonium formate / acetonitrile = 80 / 20 0 1 mL/min (6MPa), 37 deg.C, 260 nm 0 2 4 6 min 4uL (1-2ug) mAU 20 1 2 3

75 x 4.6 mm water / acetonitrile / trifluoroacetic acid = 70 / 30 / 0.1 0 1 mL/min (5MPa), 37 deg.C, 260 nm 0 2 4 min 4uL (1-2ug)

TI264E-FB06 No.TI267E

Anti-HIV Nucleosides

2 1 O HN N

N N HOCH2 O 3

200 ddI (2',3'-dideoxyinosine)

1 2 O CH3 HN

O N HOCH2 O

d4T (2',3'-didehydro-3'-deoxythymidine)

3 O CH3 HN

O N HOCH2 O

0 N3 0 2 4 6 min AZT (azidothymidine)

75 x 4.6 mm A: water / trifluoroacetic acid = 100 / 0.1 B: acetonitrile / trifluoroacetic acid = 100 / 0.1 5-30%B (0-5min), 1mL/min (5MPa), 37 deg.C, 260 nm, 2uL (0.4ug)

TI267E-FD28 No.TI288E

Verapamil

1 2 O H CO 3 CN CH3 OCH3 CCH3 CH3 H3CO C(CH2)3N(CH2)2 OCH3 CH CH 3 H H3C CH3 H H O verapamil progesterone 2

100mM ammonium acetate / acetonitrile

mAU = 70 / 30 60

100mM ammonium acetate / acetonitrile = 40 / 60

100mM ammonium acetate / acetonitrile = 40 / 60 0 0 5 10 min

150 x 4.6 mm, 1 mL/min, 37 deg.C, 260 nm, 2 uL ( 0.3-1ug )

TI288E-FL22 No.TI295E

Digitalis Glycosides in Bovine Serum

1 O 2 O O O OH CH3 H CH3 H

CH CH CH3 3 H CH3 3 H O O H OH H OH H O O H O O H H H H HO 3 digoxin HO 3 digitoxin

2 mAU 1 100

0 5 10 min

Cadenza HS-C18, 150 x 3 mm A: 10mM ammonium acetate, B: acetonitrile, 0-80%B (0-12min) 0.4 mL/min (10MPa), 37 deg.C, 220 nm, 5uL (0.5ug)

TI295E-GB08 No.TI296E

Antiepilepticums in Bovine Serum

1 H 2 H 3 O N O N O H3CH2C H3CH2C NH NH N O O CONH2 primidon phenobarbital carbamazepin

1 2 mAU 200

0 5 10 min

Cadenza HS-C18, 150 x 3 mm A: 10mM ammonium acetate, B: acetonitrile, 0-80%B (0-12min) 0.4 mL/min (10MPa), 37 deg.C, 220 nm, 5 uL (50-150ng)

TI296E-GB08 No.TI303E

Minoxidil and Metabolite

1 1 N 2 N

H2N N NH2 O minoxidil 1 2

2 1 2 N N

NH N NH2 1 2 SO3H minoxidil sulfate

mAU 1 2 100

2 1

1 2 150 x 4.6 mm A: 50mM ammonium acetate B: acetonitrile 0 0-70%B (0-14min)

0 5 10 15 min 0.8 mL/min, 37 deg.C 260 nm, 2uL (0.2-0.6ug)

TI303E-GC14 No.TI338E

LC-MS/MS Application of Marajuana and it's Metabolite in Blood

THC delta-9tetrahydrocannabinol

THC-COOH

Unison US-C18, 50 x 2 mm A: 0.1% HCOOH in water, B: 0.1% HCOOH in acetonitrile 50-90%B in 5 min, 0.5 mL/min, 28 deg. C 3200 Q Trap 0-2.3 min, ESI Negative, 2.3-5 min, ESI Positive Whole blood, SPE extraction LOD THC = 0.1ng/mL LOD THC-COOH = 0.5ng/mL

Courtesy of Massachusetts State Crime Lab., USA

TI338E-GG07 No.TI340E

Catechins and Flavonoids in Black Catechu and Chinese Scullcap

1 OH 2 OH 3 OH 4 OH OH OH OH OH HO O HO O HO O HO O OH OH

OH OH OH O OH OH OH OH OH O epigallocatechin catechin epicatechin OH EGC C EC epigallocatechin gallate OH EGCG OH OH 6 HO O 5 O OH OH O OH epicatechin gallate OH ECG

5 COOH O O O OH 4 HO HO 6 OH OH O baicalin OH 2 3 7 HO O 1 8 7 9 HO OH O scutellarein

8 HO O

HO Unison UK-C18, 250 x 4.6mm OH O baicalein A: 0.125% TFA in water B: acetonitrile OCH3 9 HO O 5-20%B (0-8min), 20-95%B (8-20min) 1.0 mL/min, 45 deg.C 5 uL inj., 2mg/40mL, UV at 280 nm OH O wogonin

Courtesy of Perrigo Co., USA

TI340E-GG24 No.TI354E

Essential Oil (Peppermint)

246 peaks

mAU 25

0 40-100%B(0-240min), 100%B(240-300min), 16MPa, 2uL

0 100 200 300 min

169 peaks mAU 25

0 40-100%B(0-120min), 100%B(120-150min), 9MPa, 1uL

0 50 100 150 min Cadenza CD-C18 A: water / trifluoroacetic acid = 100 / 0.1 B: acetonitrile / trifluoroacetic acid = 100 / 0.1 0.5mL/min, room temp., 220 nm

TI354E-GH07 No.TI355E

Essential Oils

mAU peppermint 246 peaks 200

150 sandalwood 153 peaks

eucalyptus 168 peaks 100

grapefruit 142 peaks

lavender 146 peaks

0 0 100 200 300 min

Cadenza CD-C18, 500 x 4.6 mm A: water / trifluoroacetic acid = 100 / 0.1 B: acetonitrile / trifluoroacetic acid = 100 / 0.1 40-100%B(0-240min), 100%B(240-300min) 0.5mL/min (16MPa), room temp., 220 nm, 2uL

TI355E-GH08 No.TI360E

Taurine in Nutritious Supplement Drink

O H2N CH2 CH2 S OH mV O 80 taurine

Drink A 60

20 Drink B

0 0 10 20 min

Unison UK-Amino, 100 x 3 mm A: acetonitrile, B: 100mM ammonium acetate 11%B(0-20min), 100%B(20-25min) 0.4 mL/min (3MPa), 37 deg.C, ELSD 1uL(diluted by adding 100mM ammonium acetae)

TI360E-GJ01 No.TI361E

Inositol in Nutritious Supplement Drink

OH mV HO OH 80

HO OH OH inositol

Drink A

Drink B

0 10 20 min

Unison UK-Amino, 100 x 3 mm A: acetonitrile, B: 100mM ammonium acetate 11%B(0-20min), 100%B(20-25min) 0.4 mL/min (3MPa), 37 deg.C, ELSD, 3uL

TI361E-GJ02 No.TI365E

LC-MS/MS Application of Opiates in Whole Blood

6 1: morphine 2: oxymorphone 3: hydromorphone 4: codeine 5: oxycodone 7 5 6: 6-acetyl morphine 7: hydrocodone 3 2

Unison US-C18, 50 x 2 mm

A: 0.1% HCOOH in Water B: 0.1% HCOOH in Acetonitrile 5%B (0-0.5min) 5-25%B (0.5-2.0mm) 25-90%B (2.0-3.5 min) 90%B (3.5-3.6 min) 0.6 mL/min, 28 deg. C

3200 Q-Trap, ESI Positive Whole blood, SPE Extraction LOD = 0.5ng/mL; LOQ = 1.0ng/mL

Courtesy of Massachusetts State Crime Lab., USA

TI365E-GJ09 No.TI372E

Cephem Antibiotics

COOH COOH COOH NH O NH O H2N S O 2 O N Cl 2 O N CH3 O N CH CH2 C CNH C CNH N C CNH S S S H H H H H H N OH H H

1 cefaclor 2 cefalexin 3 cefdinir

3 mV 100 1

2 normal phase

Unison UK-Amino, 50 x 3 mm acetonitrile / 50mM CH3COONH4 = 80 / 20 0 0.6mL/min (3MPa), 37deg.C 0 2 4 6 min 260nm, 0.4uL (0.05-0.3ug)

3 mV 100 reversed phase

2 1 50

Unison UK-C18, 50 x 3 mm 50mM CH3COONH4 / acetonitrile = 92 / 8 0 0.6mL/min (6MPa), 37deg.C 0 2 4 6 min 260nm, 0.4uL (0.03-0.3ug)

TI372E-GJ01 No.TI384E

Tween 20 in IgG Aqueous Solution

O O HO OH ) w( ( )x O O OH CH ( )y IgG O CH (CH ) CH O 2 2 9 3

mV ) z( O 30 Sum of w + x + y + z = 20 Tween20

Tween20 20

10 Cadenza HS-C18, 50 x 3 mm A: water, B: tetrahydrofuran 0%B(0-3min), 0-80%B(3-5min) 0 0.3 mL/min, 37 deg.C, ELSD 5 uL 0 2 4 6 8 min (IgG: 25ug, Tween20: 0.25ug)

7 R2 = 0.9054 6

log(AREA) 4

2 -2.5 -2.25 -2 -1.75 -1.5 log(Tween20/IgG)

TI384E-HA28 No.TI386E

Indomethacin in Gelatin Aqueous Solution

indomethacin

O C Cl mAU N CH3 200 H3CO CH2 C OH O indomethacin gelatin

300 th

250 th Run Pressure 100 No. N(indo) MPa 200 th 1 9300 2.6 50 10500 2.6 150 th 100 9700 2.6 150 10400 2.6 100 th 200 9900 2.6 250 9600 2.6 50 th 300 9700 2.7 1 st 0

0 1 2 min

Cadenza HS-C18, 30 x 3mm A: water /formic acid = 100 /0.1, B: acetonitrile /formic acid = 100 /0.1 0-90%B (0-2min), 0.4mL/min (3MPa), 37deg.C, 260nm 1uL (indomethacin: 0.1ug, gelatin: 5ug)

TI386E-HA31 No.TI387E

Calcitonin in Gelatin Aqueous Solution

gelatin

calcitonin

calcitonin acetate, salmon (MW 3492) mAU 100 Cys-Ser-Asn-Leu-Ser-Thr-Cys-Val-Leu- Gly-Lys-Leu-Ser-Gln-Glu-Leu-His-Lys- Leu-Gln-Thr-Tyr-Pro-Arg-Thr-Asn-Thr-

Gly-Ser-Gly-Thr-Pro-NH2 .CH3COOH

calcitonin in gelatin aqueous solution

calcitonin in water

gelatin in water 0 0 1 2 3 4 min

Cadenza HS-C18, 30 x 3mm A: water /trifluoroacetic acid = 100 /0.1 B: acetonitrile /trifluoroacetic acid = 100 /0.07 0-45%B (0-2min), 0.4mL/min (3MPa), 37deg.C, 220nm 2uL (calcitonin: 1ug, gelatin: 10ug)

TI387E-HB01 No.TI389E

Sulfamethoxazole in Alginate Aqueous Solution

sulfamethoxazole O O COONa OH HO n sodium L-guluronate O COONa O OH HO mV m 100 sodium D-mannuronate sodium alginate

H3C O N O NH S NH2 O sulfamethoxazole

sulfamethoxazole in alginate aqueous solution detection: 280nm alginate sulfamethoxazole in water detection: 280nm

alginate in water detection: ELSD 0 0 1 2 3 4min

Cadenza HS-C18, 30 x 3mm A: 10mM TFA-ammonium B: acetonitrile 0-50%B (0-2min), 0.4mL/min (3MPa), 37deg.C 0.8uL (sulfamethoxazole: 0.08ug, alginate: 0.8ug)

TI389E-HB06 No.TI390E

Lidocaine in CMC-Na Aqueous Solution O

lidocaine O NaO O

OH OH O O OH O NaO mV O

OH 100 O O OH n O NaO O OH HO OH carboxymethylcellulose sodium salt (CMC-Na)

CH3 O CH2CH3 NH C OCH2N CH2CH3 CH 50 3 CMC-Na lidocaine

lidocaine in CMC-Na aqueous solution detection: 260nm

lidocaine in water, detection: 260nm

CMC-Na in water, detection: ELSD 0

0 1 2 3 4 min

Cadenza HS-C18, 30 x 3mm A: 10mM ammonium acetate B: acetonitrile 0-70 %B (0-2min), 0.6 mL/min (5MPa), 37 deg.C 1.5 uL (lidocaine: 5ug, CMC-Na: 2ug)

TI390E-HB06 No.TI391E

Cefalexin in CMC-Na Aqueous Solution O

O cefalexin NaO O

OH OH O O OH mV O NaO 100 O

OH O O OH n O NaO O OH HO OH carboxymethylcellulose sodium salt (CMC-Na)

COOH NH O 2 O N CH3 C CNH 50 S H H H cefalexin

CMC-Na cefalexin in CMC-Na aqueous solution detection: 260nm

cefalexin in water, detection: 260nm

CMC-Na in water, detection: ELSD 0 0 1 2 3 4 min

Cadenza HS-C18, 30 x 3mm A: water /heptafluorobutryric acid = 100 /0.1 B: acetonitrile /heptafluorobutryric acid = 100 /0.1 0-70 %B (0-2min), 0.4 mL/min (3MPa), 37 deg.C 1 uL (lidocaine: 0.2ug, CMC-Na: 1ug)

TI391E-HB06 No.TI392E

Verapamil in HPC Aqueous Solution

CH2OR verapamil O OR CH3 R= H or O CH2CHO H OR n m mV hydroxypropylcellulose (HPC) 100

H CO 3 CN CH3 OCH3 H3CO C(CH2)3N(CH2)2 OCH3 CH .HCl H3C CH3 verapamil hydrochloride

HPC verapamil in HPC aqueous solution detection: 260nm

verapamil in water, detection: 260nm

HPC in water, detection: ELSD 0 0 1 2 3 min

Cadenza HS-C18, 30 x 3mm A: 10mM ammonium acetate B: acetonitrile 30-90%B (0-1.5min), 0.4mL/min (3MPa), 37deg.C 1uL (verapamil: 1ug, HPC: 1ug)

TI392E-HB07 No.TI393E

Glutathiones

H NH 2 H O 1 2 N OH HO N H NH O O H O 2 H O H N OH S HO N H O O H O S O H O HS O H N HO N OH H H NH2 O glutathione reduced (GSH) glutathione oxidized (GSSG)

1 2 mAU 50

0 2 4 6 8 min

UK-Amino, 100 x 4.6 mm A: acetonitrile, B: 50mM ammonium acetate 80-100 %B (0-8min), 1 mL/min 37 deg.C, 220 nm, 5 uL(5ug)

TI393E-HB14 No.TI395E

Disopyramide in PVP Aqueous Solution

disopyramide H2C CH

N O mV n 100 polyvinylpyrrolidone K30 (PVP)

(H3C)2HC NCH2H2CCONH2 (H3C)2HC PVP N

50 disopyramide

disopyramide in PVP aqueous solution detection: 260nm

disopyramide in water, detection: 260nm

PVP in water, detection: ELSD 0 0 1 2 3 min

Cadenza HS-C18, 30 x 3mm A: 10mM ammonium acetate B: acetonitrile 20-90%B (0-2min), 0.4mL/min (4MPa), 37deg.C 1.5 uL (disopyramide: 0.4 ug, PVP: 1.5 ug)

TI395E-HB22 No.TI398E

Basic Compounds: Antidepressant drug

10 O 1

mAU 2 1 CH3 3 CHCH2CH2N doxepine CH3

2 pKa = 10.4 N H 5 CH2 CH2 CH2 N 6 desipramine CH3 4 5 3 pKa = 9.5 N CH3 CH2 CH2 CH2N imipramine CH3

0 4 pKa = 9.7 0 5 10 15 min H CHCH2CH2N nortriptyline CH3 10 2

mAU 3 5 pKa = 9.4 1 CH3 CHCH2CH2N amitriptyline CH3

6 5 6 N CH3 CH2 CHCH2N 4 5 CH3 CH3 trimipramine

150 x 3mm

0 water /acetonitrile /formic acid = 70 /30 /0.1 0.5 mL/min, 37 degC, 10-12 MPa 0 5 10 15 min 260 nm, 1 uL (0.1 mg/mL)

TI398E-HC10 No.TI399E

Polypeptide Antibiotic

CH3 NH2 H3C O O H HO O N HN H HN O S CH3 O H H O H CH O N N N N 3 HN N NH H O H O NH2 N H3C H3C O CH3 CH3 O NH O O NH HO HN O

NH2 bacitracin MW =1422

mAU 75 x 4.6 mm 50 water /acetonitrile /TFA = 80 /20 /0.1 1mL/min, 37degC, 260nm, 2uL (1 mg/mL)

0 2 4 6 8 10 min

TI399E-HC10 No.TI402E

Voglibose, Acarbose

1 CH2OH OH OH HO NH 1 HO OH voglibose OH

CH2OH CH3 CH2OH CH2OH 2 O O O OH OH OH OH OH HO N O O HO H OH OH OH 1 acarbose 2 mV 100

Unison UK-Amino, 250 x 3 mm 0.4 mL/min (7 MPa), 1 uL (2 ug) 50

Unison UK-Amino, 250 x 4.6 mm 1 mL/min (9 MPa), 2 uL (4 ug) 0 0 5 10 min

acetonitrile /50mM ammonium acetate = 70 /30 60 deg.C, ELSD

TI402E-HC18 No.TI409E

5-Fluorouracil and Related Compounds

3 1 O 2 O F F 2 HN HN 4 O N O N H H dihydrofluorouracil 5-fluorouracil mAU 1 100 3 O 4 O HN HN

O N O N H H dihydrouracil uracil 50 normal phase

Unison UK-Amino, 250 x 3 mm hexane /tetrahydrofuran /water /TFA = 15 /83 /2 /0.15 0 0.4 mL/min (6MPa), 60 deg.C, 210 nm 0 5 10 min 2.5 uL (0.3-1.4ug, diluted with eluent)

4 2 3 mAU 100

reversed phase

Unison UK-Phenyl, 250 x 4.6 mm 10 mM TFA-ammonium 0 0.8 mL/min (13 MPa), 37 deg.C, 210 nm 0 5 10 min 0.8 uL (0.2-0.4ug)

TI409E-HD28 No.TI410E

Tetracycline antibiotics

OH O OH O O OH O OH O O OH O OH O O OH OH OH NH2 NH2 NH2 OH OH OH HO OH N HO N Cl HO N oxytetracycline (OTC) tetracycline (TC) chlortetracycline (CTC)

Cadenza CW-C18, 150 x 4.6 mm water /acetonitrile /HCOOH = 80 /20 /0.1 1 mL/min, 40 deg.C, 260 nm, 20 uL (1ppm)

Courtesy of Mr. N. MAEDA, ASSOCIATION OF MEAT SCIENCE & TECHNOLOGY INSTITUTE

TI410E-GE08 No.TI411E

LC-MS/MS Application -Tetracycline Antibiotics

20080509_OTC_02 MRM of 6 Channels ES+ 7.29 100 7.98 TIC 7.07 3.04e4 % 0 2.50 5.00 7.50 10.00 12.50 15.00 17.50 20080509_OTC_02 MRM of 6 Channels ES+ OH O OH O O 7.98 OH 100 479.27 > 444 1.27e4 NH2 7.68 % first ion CTC OH 0 Cl HO N 2.50 5.00 7.50 10.00 12.50 15.00 17.50 20080509_OTC_02 MRM of 6 Channels ES+ 7.98 chlortetracycline 100 479.27 > 154.1 CTC second ion 8.82e3 (CTC) % 0 2.50 5.00 7.50 10.00 12.50 15.00 17.50 20080509_OTC_02 MRM of 6 Channels ES+ OH OH 7.07 O O O 100 461.31 > 426.15 OH 1.97e4 OTC first ion NH2 % OH 0 HO 2.50 5.00 7.50 10.00 12.50 15.00 17.50 OH N 20080509_OTC_02 MRM of 6 Channels ES+ 7.07 oxytetracycline 100 461.31 > 201.2 OTC second ion 2.52e3 (OTC) % 0 2.50 5.00 7.50 10.00 12.50 15.00 17.50 20080509_OTC_02 MRM of 6 Channels ES+ 7.29 100 445.36 > 410.1 1.74e4 OH OH 6.94 TC first ion O O O

% OH 0 NH2 2.50 5.00 7.50 10.00 12.50 15.00 17.50 OH 20080509_OTC_02 MRM of 6 Channels ES+ HO N 7.33 100 445.36 > 154.1 TC second ion 1.20e4 tetracycline % 0 Time (TC) 2.50 5.00 7.50 10.00 12.50 15.00 17.50

Cadenza CW-C18, 100 x 2 mm + Guard column A: 0.1% HCOOH aq., B: 0.1% HCOOH in ACN 5 - 95%B ( 0 - 7 min ), 95 - 5%B ( 7 - 8 min ), 5%B ( 8 - 17 min ) 0.2 mL/min, 40 deg.C, 10 uL ( 20 ppb ), ESI, positive

Courtesy of Mr. N. MAEDA, ASSOCIATION OF MEAT SCIENCE & TECHNOLOGY INSTITUTE, JAPAN

TI411E-HF24 mV 1000

500

0 2 4 6 8 min

No.TI422E

Simultaneous analysis of drug substance and lactose mV 60

2 O 1 HN N mV 500 H2N N N CH2OCH2CH2OH 1 acyclovir (0.1ug) mAU 60

40 CH2OH 2 O OH OH 40 CH2OH O HO O OH OH

ELSD OH 0 lactose (10ug) 20

20 260nm 0 0 2 4 6 min

Unison UK-Amino, 50 x 3 mm A: acetonitrile, B: water 1-100%B(0-5min) 0.4 mL/min (2MPa), 37 deg.C 1.6 uL (0.1, 10ug)

0 TI422E-HK01 0 2 4 6 8 min No.TI426E

Aminoglycoside Antibiotics

NH NH HN NH 1 2 H N NH2 1 OH HO O OH O 3 CHO H3C 2 .11/2H2SO4 OH O

HO O CH2OH 4 H3CHN

OH Cadenza CW-C18 streptomycin sulfate 5

CH2OH O NH2 2 HO O mV OH CH2NH2 O 100 .2H2SO4 OH HO O OH OH OH N H NH2 Cadenza CD-C18 NH2 O amikacin disulfate

CH2OH O NH2 3 HO O OH CH2NH2 O .H2SO4 OH HO O OH 50 Unison UK-C18 OH NH2 NH2 kanamycin sulfate

CH2OH O 4 NH2 HO O OH CH2NH2 O .xH2SO4 Cadenza CL-C18 HO O H2N OH NH2 NH2 0 tobramycin sulfate 0 10 20 30 min HO O C : R = CH 5 NHCH3 1 1 3 H3C O R2 R2 = NHCH3 250 x 3 mm OH R1 CH C2 : R1 = CH3 A: water /heptafluorobutyric acid = 100 /0.1 O R2 = NH2 O B: acetonitrile /heptafluorobutyric acid = 100 /0.1 H2N C : R = H OH 2b 1 20-34%B(0-35min) .H2SO4 NH 2 R2 = NHCH3 NH2 0.4 mL/min(13-16MPa) , 37 deg.C, ELSD, 2 uL(4ug) gentamicin sulfate

TI426E-HH11 No.TI427E

Polypeptide Antibiotic (2)

OH H2N H3C O O NH2 NH2 N N

H O H O NH H O H N N H2N N N R

O H O H O CH3 NH HN HO CH3 O mAU H H 40 H3C N N .H2SO4 O O NH H3C 2 B1: R = CH3, MW 1302 B2: R = H, MW 1288 Polymyxin B

0 5 10 15 min

75 x 3 mm water /acetonitrile /trifluoroacetic acid = 75 /25 /0.1 0.4 mL/min(6-8MPa), 37degC, 220nm, 1.6 uL (3ug)

TI427E-HH12 No.TI428E

Antibiotic (Erythromycin)

O CH3 H3C CH3 O OH H HO CH3 OH CH3 N H3C H3C OH O O CH3 CH3 H3C OH O H O CH O CH3 3 O CH3 erythromycin mAU 10

Cadenza CD-C18

Cadenza CW-C18 0

0 5 10 min

150 x 4.6 mm, 20mM HCOONH4 /acetonitrile = 65 / 35 1 mL/min (11-13MPa), 37 deg.C, 210 nm, 5 uL(10ug)

TI428E-HH04 No.TI434E

Antibiotic (Rifampicin)

HO O O OH O OH OH H3CO NH N O N OH N O O rifampicin mAU 60

0 0 2 4 6 8 min

75 x 3 mm A: water / formic acid = 100 / 0.1 B: acetonitrile / formic acid = 100 / 0.1 40-90 %B (0-8min), 0.4 mL/min 37 deg.C, 260 nm, 0.4 uL (0.4ug)

TI434E-HI01 No.TI435E

Antibiotic (Tylosin)

O O

O CH3 O O O O OH tylosin HO CH3 H3CO OCH3 O CH3 N CH3 HO O O CH3 OH OH

CH3 mAU

200

100

0 2 4 6 8 min

75 x 3 mm A: water / formic acid = 100 / 0.1 B: acetonitrile / formic acid = 100 / 0.1 25-70 %B (0-8min), 0.4 mL/min 37 deg.C, 260 nm, 2 uL (2ug)

TI435E-HI01 No.TI436E

Antibiotic (Vancomycin)

OH HO H N 2 CH3 H3C O OH HO O O Cl O Cl O O OH vancomycin O O O H H H H N H N O N N N N H HN O H2N O O O HO OH HO OH mAU

200

100

0 0 2 4 6 8 min

75 x 3 mm A: water / formic acid = 100 / 0.1 B: acetonitrile / formic acid = 100 / 0.1 5-70 %B (0-8min), 0.4 mL/min 37 deg.C, 260 nm, 2 uL (2ug)

TI436E-HI01 No.TI463E

LC-MS/MS Application for Duloxetine and Ethyl Morphine in Whole Blood

XIC of +MRM (4 pairs): 298.2/44.1 amu from Sample 3 (1.0) of 1009.wiff (Turbo Spray) Max. 3890.0 cps.

7570 3.09

.. TIC I. 2.83 2.94 0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 38 74 111 147 184 220 257 294 330 Time, min XIC of +MRM (4 pairs): 298.2/44.1 amu from Sample 3 (1.0) of 1009.wiff (Turbo Spray) Max. 3890.0 cps.

3.09 3890 Duloxetine ..

I. 2.83 2.94 0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 38 74 111 147 184 220 257 294 330 Time, min XIC of +MRM (4 pairs): 298.2/154.3 amu from Sample 3 (1.0) of 1009.wiff (Turbo Spray) Max. 1395.0 cps.

3.09 1000 Duloxetine .. I. 0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 38 74 111 147 184 220 257 294 330 Time, min XIC of +MRM (4 pairs): 314.2/152.2 amu from Sample 3 (1.0) of 1009.wiff (Turbo Spray) Max. 7570.0 cps.

2.23 7570

.. Ethyl morphine I. 0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 38 74 111 147 184 220 257 294 330 Time, min XIC of +MRM (4 pairs): 314.2/128.3 amu from Sample 3 (1.0) of 1009.wiff (Turbo Spray) Max. 5875.0 cps.

2.23 5000

. Ethyl morphine I.. 0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 38 74 111 147 184 220 257 294 330 Time, min

Unison US-C18, 50 x 2 mm

A: 0.1% HCOOH in water, B: 0.1% HCOOH in acetonitrile 5%B (0-0.5min), 5-90%B (0.5-4.5min), 5%B (4.5-6min) 0.5mL/min (LOD 0.05 ng/mL, LOQ 0.1 ng/mL)

Whole Blood, SPE Extraction 3200 Q-Trap: ESI, MRM Positive Duloxetine: m/z 298.1 -> 44.1 and 154.3 Ethyl Morphine (I.S.): m/z 314.2 -> 152.2 and 128.3

Ref) Rapid Quantification of Duloxetine in Blood and Urine by LC-ESI-MS/MS Albert Elian, Massachussetts State Police Crime Lab, USA Society of Forensic Toxicologists (SOFT), 2008, USA

Courtesy of Massachusetts State Police Crime Lab., USA

TI463E-HL10 No.TI494E

Betamethasone (Antihistamine:Adrenal corticosteroid)

CH2OH 1 C O H C HO 3 OH 1 Unison UK-Phenyl CH3 75 x 4.6 mm H3C H water / acetonitrile F H / trifluoroacetic acid O = 72 / 28 / 0.1 betamethasone 1 Unison UK-Phenyl, 75 x 4.6 mm water / acetonitrile / trifluoroacetic acid = 68 / 32 / 0.1 1 Unison UK-C8, 75 x 4.6 mm mAU water / acetonitrile / trifluoroacetic acid 120 = 70 / 30 / 0.1 1 Unison UK-C8, 75 x 4.6 mm water / acetonitrile / trifluoroacetic acid = 68 / 32 / 0.1 1 Cadenza CD-C18, 75 x 4.6 mm 80 water / acetonitrile / trifluoroacetic acid = 68 / 32 / 0.1 1 Cadenza CL-C18, 75 x 4.6 mm water / acetonitrile / trifluoroacetic acid = 68 / 32 / 0.1 1 40 Unison UK-C18, 75 x 4.6 mm water / acetonitrile / trifluoroacetic acid = 68 / 32 / 0.1

1 Unison US-C18, 150 x 4.6 mm water / acetonitrile / trifluoroacetic acid = 68 / 32 / 0.1 0 0 5 10 min

1 mL/min (4-5MPa), 37 deg.C, 260 nm, 1 uL (0.25ug, DMSO)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI494E-IL17 North America Other Countries No.TI495E

Mequitazine (Antihistamine) 1 N

1 Unison UK-Phenyl 75 x 4.6 mm N water / acetonitrile S / trifluoroacetic acid = 64 / 36 / 0.1 mequitazine 1 Unison UK-Phenyl, 75 x 4.6 mm water / acetonitrile / trifluoroacetic acid = 60 / 40 / 0.1 1 Unison UK-C8, 75 x 4.6 mm water / acetonitrile / trifluoroacetic acid = 62 / 38 / 0.1 mAU 1 800 Unison UK-C8, 75 x 4.6 mm water / acetonitrile / trifluoroacetic acid = 60 / 40 / 0.1 1 Cadenza CD-C18, 75 x 4.6 mm water / acetonitrile / trifluoroacetic acid = 60 / 40 / 0.1 400 1 Cadenza CL-C18, 75 x 4.6 mm water / acetonitrile / trifluoroacetic acid = 60 / 40 / 0.1 1 Unison UK-C18, 75 x 4.6 mm water / acetonitrile / trifluoroacetic acid = 60 / 40 / 0.1 0

0 2 4 6 8 min

1 mL/min (5-6MPa), 37 deg.C, 260 nm, 1 uL (1ug, DMSO)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI495E-IL16 North America Other Countries No.TI496E

Menatetrenone (Vitamin K)

1 1 O CH3 CH3 CH2CH CCH2 H Unison UK-Phenyl O 4 75 x 4.6 mm menatetrenone water / acetonitrile = 28 / 72 1

Unison UK-C8, 75 x 4.6 mm water / acetonitrile = 15 / 85 1

mAU Unison UK-C18, 75 x 4.6 mm water / acetonitrile = 2 / 98 200 1

Cadenza CL-C18, 75 x 4.6 mm water / acetonitrile = 2 / 98

100 Cadenza CD-C18, 75 x 4.6 mm water / acetonitrile = 2 / 98

Unison US-C18, 150 x 4.6 mm water / acetonitrile = 2 / 98 0

0 5 10 min

1 mL/min (3-6MPa), 37 deg.C, 260 nm, 1 uL (3ug, DMSO)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI496E-IL16 North America Other Countries No.TI497E

Furosemide (Diuretic)

1 H 1 Cl N Unison UK-Phenyl O O 75 x 4.6 mm H2N S O water / acetonitrile O OH / formic acid = 69 / 31 / 0.1 furosemide 1 Unison UK-Phenyl, 75 x 4.6 mm water / acetonitrile / formic acid = 67 / 33 / 0.1

Unison UK-C8, 75 x 4.6 mm water / acetonitrile / formic acid = 67 / 33 / 0.1 mAU 1 400 Cadenza CL-C18, 75 x 4.6 mm water / acetonitrile / formic acid = 67 / 33 / 0.1

Cadenza CD-C18, 75 x 4.6 mm water / acetonitrile / formic acid = 67 / 33 / 0.1 200 1

Unison UK-C18, 75 x 4.6 mm water / acetonitrile / formic acid = 67 / 33 / 0.1

1 Unison US-C18, 150 x 4.6 mm water / acetonitrile / formic acid 0 = 67 / 33 / 0.1

0 2 4 6 8 10 min

1 mL/min (4-6MPa), 37 deg.C, 260 nm, 1 uL (1ug, DMSO)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI497E-IL16 North America Other Countries No.TI498E

Naftopidil (alpha1-receptor blocker)

1 1 OH O N N Unison UK-Phenyl 75 x 4.6 mm O 20mM ammonium acetate naftopidil CH3 / acetonitrile = 54 / 46 1 Unison UK-Phenyl, 75 x 4.6 mm 20mM ammonium acetate / acetonitrile = 42 / 58 1 Unison UK-C8, 75 x 4.6 mm 20mM ammonium acetate / acetonitrile = 50 / 50 1

mAU Unison UK-C8, 75 x 4.6 mm 20mM ammonium acetate / acetonitrile = 42 / 58 200 1 Cadenza CD-C18, 75 x 4.6 mm 20mM ammonium acetate / acetonitrile = 42 / 58 1 Unison UK-C18, 75 x 4.6 mm 20mM ammonium acetate / acetonitrile = 42 / 58 100 1 Cadenza CL-C18, 75 x 4.6 mm 20mM ammonium acetate / acetonitrile = 42 / 58 1 Unison US-C18, 150 x 4.6 mm 20mM ammonium acetate / acetonitrile = 42 / 58 0

0 5 10 min

1 mL/min (6-8MPa), 37 deg.C, 260 nm, 1 uL (1ug, DMSO)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI498E-IL14 North America Other Countries No.TI499E

Pranoprofen (Nonsteroid anti-inflammatory drug:NSAID)

1 Unison UK-Phenyl 1 CH3 75 x 4.6 mm CH C OH water / acetonitrile / formic acid N O O = 72 / 28 / 0.1 pranoprofen 1 Unison UK-Phenyl, 75 x 4.6 mm water / acetonitrile / formic acid = 69 / 31 / 0.1 1 Unison UK-C8, 75 x 4.6 mm water / acetonitrile / formic acid = 70 / 30 / 0.1 1

mAU Unison UK-C8, 75 x 4.6 mm water / acetonitrile / formic acid = 69 / 31 / 0.1 400 1 Cadenza CD-C18, 75 x 4.6 mm water / acetonitrile / formic acid = 69 / 31 / 0.1 1 Cadenza CL-C18, 75 x 4.6 mm water / acetonitrile / formic acid 200 = 69 / 31 / 0.1 1 Unison UK-C18, 75 x 4.6 mm water / acetonitrile / formic acid = 69 / 31 / 0.1

1 Unison US-C18, 150 x 4.6 mm water / acetonitrile / formic acid = 69 / 31 / 0.1 0 0 5 10 min

1 mL/min (4-6MPa), 37 deg.C, 260 nm, 1 uL (1ug, DMSO)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI499E-IL14 North America Other Countries No.TI506E

Codeine phosphate (Narcotic antitussive) CH3 1 N

1 Unison UK-Phenyl 75 x 4.6 mm water / acetonitrile O O OH / trifluoroacetic acid CH3 - H3PO4 - 1/2 H2O = 91 / 9 / 0.1 codeine phosphate 1 Unison UK-Phenyl, 75 x 4.6 mm

mAU water / acetonitrile / trifluoroacetic acid = 89 / 11 / 0.1 1 Unison UK-C8, 75 x 4.6 mm water / acetonitrile / trifluoroacetic acid 60 = 90 / 10 / 0.1 1 Unison UK-C8, 75 x 4.6 mm water / acetonitrile / trifluoroacetic acid = 89 / 11 / 0.1 1 Cadenza CD-C18, 75 x 4.6 mm 40 water / acetonitrile / trifluoroacetic acid = 89 / 11 / 0.1 1 Cadenza CL-C18, 75 x 4.6 mm water / acetonitrile / trifluoroacetic acid = 89 / 11 / 0.1 1 20 Unison UK-C18, 75 x 4.6 mm water / acetonitrile / trifluoroacetic acid = 89 / 11 / 0.1

1 Unison US-C18, 150 x 4.6 mm water / acetonitrile / trifluoroacetic acid = 89 / 11 / 0.1 0

0 5 10 min

1 mL/min (4-6MPa), 37 deg.C, 260 nm, 2 uL (2ug, DMSO)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI506E-IL14 North America Other Countries No.TI507E

Zopiclone (Nonbenzodiazepine hypnotic)

1 1 O N N Cl N N O Unison UK-Phenyl 75 x 4.6 mm O N N CH3 20mM ammonium acetate / acetonitrile = 71 / 29 zopiclone 1 Unison UK-Phenyl 75 x 4.6 mm 20mM ammonium acetate / acetonitrile = 70 / 30

mAU 1 Unison UK-C8, 75 x 4.6 mm 120 20mM ammonium acetate / acetonitrile = 70 / 30 1 Cadenza CD-C18, 75 x 4.6 mm 20mM ammonium acetate / acetonitrile = 70 / 30 80 1 Unison UK-C18, 75 x 4.6 mm 20mM ammonium acetate / acetonitrile = 70 / 30 1 , 75 x 4.6 mm 40 Cadenza CL-C18 20mM ammonium acetate / acetonitrile = 70 / 30 1 Unison US-C18, 150 x 4.6 mm 20mM ammonium acetate / acetonitrile = 70 / 30 0

0 5 10 min

1 mL/min (5-6MPa), 37 deg.C, 260 nm, 1 uL (1ug, DMSO)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI507E-IL11 North America Other Countries No.TI508E

Rilmazafone HCl (Benzodiazepine hypnotic)

1 O CH3 1 Unison UK-Phenyl N CH 75 x 4.6 mm N 3 N H 20mM ammonium acetate N / acetonitrile = 72 / 28 N NH2 O O 1 Unison UK-Phenyl Cl - HCl - 2H2O 75 x 4.6 mm Cl 20mM ammonium acetate / acetonitrile = 70 / 30 1 Unison UK-C8 rilmazafone HCl 75 x 4.6 mm 20mM ammonium acetate / acetonitrile = 71 / 29 1 Unison UK-C8, 75 x 4.6 mm 20mM ammonium acetate / acetonitrile mAU = 70 / 30 200 1 Cadenza CD-C18, 75 x 4.6 mm 20mM ammonium acetate / acetonitrile = 70 / 30 1 Unison UK-C18, 75 x 4.6 mm 20mM ammonium acetate / acetonitrile = 70 / 30 100 1 Cadenza CL-C18, 75 x 4.6 mm 20mM ammonium acetate / acetonitrile = 70 / 30 1 Unison US-C18, 150 x 4.6 mm 20mM ammonium acetate / acetonitrile = 70 / 30 0

0 5 10 min

1 mL/min (5-6MPa), 37 deg.C, 260 nm, 1 uL (1ug, DMSO)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI508E-IL11 North America Other Countries No.TI509E

Paroxetine HCl (Antidepressant)

1 F NH

O 1 - HCl - 1/2H2O O O paroxetine - HCl

Unison UK-Phenyl 75 x 4.6 mm 1 Unison UK-C8 75 x 4.6 mm 1

Cadenza HS-C18 mAU 75 x 4.6 mm 30 1

Cadenza CW-C18 75 x 4.6 mm 1 Cadenza CD-C18 75 x 4.6 mm 1 Unison UK-C18 75 x 4.6 mm 0 0 5 10 min

50mM ammonium formate / acetonitrile = 70 / 30 1 mL/min (6-7MPa), 37 deg.C, 260 nm, 2 uL (2ug, DMSO)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI509E-IL10 North America Other Countries No.TI510E

Oseltamivir phosphate (Anti-flu medicine)

O H2N 1 O O N H O - H3PO4

oseltamivir phosphate

1 Unison UK-Phenyl 75 x 4.6 mm

mAU Unison UK-C8 75 x 4.6 mm 200 1 Cadenza CL-C18 75 x 4.6 mm

1 Cadenza CD-C18 75 x 4.6 mm 100 Unison UK-C18 75 x 4.6 mm 1 Unison US-C18 150 x 4.6 mm 0 0 5 10 min

water / acetonitrile / trifluoroacetic acid = 74 / 26 / 0.1 1 mL/min (4-5MPa), 37 deg.C, 220 nm, 1 uL (1ug, DMSO)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI510E-IL10 North America Other Countries No.TI511E

Zanamivir (Anti-flu medicine)

OH 1 OH O HO O O OH N NH2 1 H NH xH2O NH zanamivir hydrate mAU

Unison UK-Silica, 150 x 3 mm 100 A: acetonitrile / formic acid = 100 / 0.1 B: water / formic acid = 100 / 0.1 15-40 %B (0-10min) 0.4 mL/min (4MPa), 37 deg.C, 260 nm 2 uL (2ug, DMSO)

Unison UK-Amino, 150 x 3 mm 1 acetonitrile / 20mM ammonium formate 50 = 70 / 30 0.4 mL/min (5MPa), 37 deg.C, 260 nm 2 uL (2ug, DMSO)

1 Unison UK-C18, 150 x 3 mm water / formic acid = 100 / 0.1 0.4 mL/min (8MPa), 37 deg.C, 260 nm 2 uL (2ug, DMSO) 0

0 5 10 min

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI511E-IL10 North America Other Countries No.TI521E

Glutathiones

1 H NH2 O mV 2 H N OH HO N H 100 O O H O HS glutathione reduced (GSH)

1 2 H NH 2 H O N OH HO N H O O H O S S O O H O 50 H N HO N OH H H NH2 O glutathione oxidized (GSSG)

50 x 3 mm A: 5mM ammonium acetate B: 100mM ammonium acetate / ACN = 50 / 50 0 0-100 %B (0-5min), 0 %B (5-10min) 0.4 mL/min (3MPa), 37 deg.C, ELSD 0 2 4 6 min 2 uL (2ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI521E-IF17 North America Other Countries No.TI525E

Basic compounds: Antidepressant drugs

1 4 5 water /acetonitrile /formic acid 1 O = 73 /27 /0.1 2 3 CH3 CHCH2CH2N 6 CH3 doxepine pKa = 9.0

1 4 2 N 5 H water /acetonitrile /acetic acid CH2 CH2 CH2 N CH3 2 3 = 73 /27 /2

mAU desipramine pKa = 10.4

40 6 3 N CH3 4 CH2 CH2 CH2N 1 CH3 5 imipramine pKa = 9.5 10mM ammonium formate 3 2 /acetonitrile = 67 /33 4 6 H CHCH2CH2N 20 CH3 nortriptyline pKa = 9.7 3, 4 10mM ammonium acetate 1 5 5 /acetonitrile = 60 /40 CH3 CHCH2CH2N 2 CH3 amitriptyline pKa = 9.4 6

0 6 0 5 10 15 min N CH3 CH2 CHCH2N CH3 Scherzo SM-C18, 150 x 3 mm CH3 trimipramine pKa = 8.0 0.4 mL/min (9-11MPa), 37 deg.C, 240 nm 0.6 uL (120ng)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI525E-IG22 North America Other Countries No.TI531E

Chlorpheniramine maleate

2 1 A: 50mM formic acid : HOOC COOH 50mM ammonium formate C C 1 = 9 : 1, pH 2.8 H H

maleic acid 2

1 A: 50mM formic acid : 50mM ammonium formate = 8 : 2, pH 3.1 2 N CH3 CH2CH2 N 2 C CH H 3 1 A: 50mM formic acid : Cl

mAU 50mM ammonium formate dl-chlorpheniramine = 6 : 4, pH 3.5 2 500 1

A: 50mM formic acid : 50mM ammonium formate = 4 : 6, pH 3.8 2 1 A: 50mM formic acid : 50mM ammonium formate = 2 : 8, pH 4.2 Scherzo SM-C18 2 50 x 3 mm 1 A: formate buffer A: 50mM formic acid : B: acetonitrile 50mM ammonium formate 0-70 %B (0-7min) = 1 : 9, pH 4.7 0.4 mL/min (5MPa) 0 37 deg.C, 240 nm 0 2 4 6 8 min 2 uL (2ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI531E-IG23 North America Other Countries No.TI532E

Tipepidine hibenzate

2 CH mAU 1 3 2000 N 1 A: 50mM formic acid S pH 2.5 S 1 2 A: 50mM formic acid : tipepidine 50mM ammonium formate = 6 : 4, pH 3.5 1 2 A: 50mM formic acid : 2 50mM ammonium formate HO O = 4 : 6, pH 3.8 O 1 2 A: 50mM formic acid : OH 50mM ammonium formate = 2 : 8, pH 4.2 hibenzic acid 1000 1 2 A: 50mM formic acid : 50mM ammonium formate = 1 : 9, pH 4.7 2 1 A: 50mM formic acid : 50mM ammonium formate = 5 : 95, pH 4.9 2 1 A: 50mM formic acid : 50mM ammonium formate Scherzo SM-C18 = 2 : 98, pH 5.4 50 x 3 mm 2 A: 50mM ammonium formate A: formate buffer 1 pH 6.8 B: acetonitrile 20-60 %B (0-8min) 0.4 mL/min (6-8MPa) 0 37 deg.C, 280 nm 0 2 4 6 8 min 0.6 uL (1.2ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI532E-IH12 North America Other Countries No.TI533E

Clemastine fumarate

Cl 1 2 H3C H3C HOOC H N O C C H COOH fumaric acid clemastine

2 mAU 400

200 1

0 2 4 6 8 min

50 x 3 mm A: 50mM formic acid : 50mM ammonium formate = 4 : 6, pH 3.8 B: acetonitrile, 40-70 %B (0-8min), 0.4 mL/min (7MPa) 37 deg.C, 230 nm, 0.6 uL (1.2ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI533E-IH12 North America Other Countries No.TI534E

Hydroxyzine pamoate

N H N OH 2 Cl O

hydroxyzine mAU

100 2 COOH 1 OH CH2 OH

COOH

pamoic acid

2 1

50 x 3 mm A: 100mM ammonium formate 0 B: acetonitrile 40-70 %B (0-8min) 0.4 mL/min (8MPa), 37 deg.C 0 2 4 6 8 min 235 nm, 1 uL (0.1ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI534E-IG04 North America Other Countries No.TI535E

Nojirimycin relative compounds

3 1 CH2OH N SO3H mV OH H HO 40 OH nojirimycin bisulfite 2

2 CH2OH NH OH HO .HCl OH 1-deoxynojirimycin hydrochloride

20 3 CH2OH NH OH HO HO .HCl

1 1-deoxymannojirimycin hydrochloride

Scherzo SM-C18, 250 x 4.6 mm A: 5mM ammonium acetate B: 200mM ammonium acetate / acetonitrile = 80 / 20 0 -40 %B (0-10min) 0 0.5 mL/min (7MPa), 37 deg.C ELSD (spray chamber 50 deg.C, drift tube 100 deg.C) 0 5 10 min 5 uL (1.25-2.5ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI535E-IH03 North America Other Countries No.TI536E

Methimazole and potential metabolites

O 1 2

mAU H3C N NH 100 O N-methylhydantoin

4 2 H3C N N

SH methimazole 50 3 1

3 H N NH2

S N-methylthiourea

4 0 HN N 0 5 10 15 min SH Unison UK-Amino, 250 x 3 mm 2-mercaptoimidazole A: acetonitrile, B: 10mM ammonium formate 1-25 %B (0-15min) 0.4 mL/min (5MPa), 50 deg.C, 230 nm 2.4 uL (0.07-0.35 ug, diluted with ethanol)

Courtesy of Takeo Sakuma, Ph.D, MDS Analytical Technologies (SCIEX), Canada Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI536E-IH12 North America Other Countries No.TI537E

Aminoglycoside antibiotics

NH CH2OH CH2OH CH2OH 1 NH 2 O 3 O 4 O 2HN NH H NH2 NH2 NH2 N NH2 HO O HO O HO O OH HO OH OH OH O CH2NH2 CH2NH2 CH2NH2 OH O O .H2SO4 O .xH2SO4 O .2H2SO4 OH OH CHO O O O H3C HO HO HO .11/2H2SO4 OH OH H2N OH O OH OH OH OH N NH2 NH2 HO O H NH2 CH2OH NH2 O NH2 NH2 H3CHN

OH amikacin disulfate kanamycin sulfate tobramycin sulfate streptomycin sulfate 5 HO O NHCH3 C : R = CH H3C O 1 1 3 R2 OH R1 CH R2 = NHCH3 O C2 : R1 = CH3 O R2 = NH2 H2N OH C2b: R1 = H .H2SO4 NH2 NH2 R2 = NHCH3 gentamicin sulfate mV 2 40 1

5 4

0 10 20 min

Scherzo SM-C18, 150 x 3 mm A: 5mM acetic acid : 5mM ammonium acetate = 1 : 1, pH 4.7 B: (200mM acetic acid : 200mM ammonium acetate = 1 : 1, pH 4.7) / acetonitrile = 70 / 30 0-100 %B (0-20min), 0.4 mL/min (8MPa), 37 deg.C ELSD (spray chamber 50 deg.C, drift tube 100 deg.C), 1 uL (5 ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI537E-IH17 North America Other Countries No.TI543E

Benzalkonium chloride

CH3 mV + 60 CH2 N R Cl- CH3

benzalkonium chloride

0 0 5 10 min

150 x 3 mm A: 10mM nitric acid B: methanol / 1M nitric acid = 100 / 1 70-100 %B (0-10min) 0.4 mL/min (12-13MPa), 37 deg.C, 260 nm, 3 uL (15 ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI543E-II14 North America Other Countries No.TI544E

Benzethonium chloride

CH3 CH3 CH3 + H3C C CH2 C (OCH2CH2)2 N CH2 - CH3 CH3 CH3 Cl benzethonium chloride

mV 100

0 0 5 10 min

150 x 3 mm A: 10mM nitric acid B: methanol / 1M nitric acid = 100 / 1 70-100 %B (0-10min) 0.4 mL/min (12-13MPa), 37 deg.C, 260 nm, 1.6 uL (8 ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI544E-II14 North America Other Countries No.TI545E

Anti-hyperlipidemic drug in bovine serum (probucol)

1 (CH3)3C CH3 C(CH3)3

HO S C S OH

(CH3)3C CH3 C(CH3)3 probucol mAU

0 5 10 min

Cadenza HS-C18, 150 x 3 mm A: 50mM ammonium formate, B: acetonitrile 0-80 %B (0-10min), 0.5 mL/min (14MPa) 37 deg.C, 280 nm, 5 uL (0.5ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI545E-II16 North America Other Countries No.TI568E

Carboxymethylcellulose O

O HO O

OH OH O O OH O mV HO 100 O

OH O O OH n O HO O + OH Na HO OH carboxymethylcellulose sodium salt (ca.100 kDa)

0 5 10 min

Presto FF-C18, 150 x 4.6mm A: water / trifluoroacetic acid = 100 / 0.1 B: acetonitrile / trifluoroacetic acid = 100 / 0.1 5-60 %B (0-10min), 0.4 mL/min (23MPa), 37 deg.C ELSD (spray chamber 50deg.C, drift tube 100deg.C) 8 uL (16ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI568E-JA15 North America Other Countries No.TI569E

Hydroxypropylcellulose

CH2OR O CH3 OR R= H or CH2CHO H O m OR n hydroxypropylcellulose (55 ~ 70 kDa)

mV 100

0 0 5 10 15 min

Presto FF-C18, 150 x 4.6mm A: water B: acetonitrile 5-90 %B (0-15min), 0.4 mL/min (21MPa), 37 deg.C ELSD (spray chamber 50deg.C, drift tube 100deg.C), 2 uL (10ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI569E-JA15 North America Other Countries No.TI570E

Polyvinylpyrrolidone (PVP)

H2C CH

N O n polyvinylpyrrolidone (ca.50 kDa)

mV 50

0 5 10 15 min

Presto FF-C18, 150 x 4.6mm A: water / trifluoroacetic acid = 100 / 0.1 B: acetonitrile / trifluoroacetic acid = 100 / 0.1 20-60 %B (0-10min), 0.4 mL/min (23MPa), 37 deg.C ELSD (spray chamber 50deg.C, drift tube 100deg.C), 1 uL (5ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI570E-JB12 North America Other Countries No.TI592E

Cetirizine (Antihistamine)

N H N OH 1 Cl O cetirizine O mAU

400 1

0 5 10 15 min

150 x 4.6 mm 100mM ammonium formate / acetonitrile = 67 / 33 1 mL/min (9-12MPa), 37 deg.C, 240 nm 2 uL (2 ug, DMSO)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI592E-JC12 North America Other Countries No.TI593E

Plerixafor (Chemokine receptor antagonist)

H H N N

HN N N NH

N N H H plerixafor 1

mV 20

ELSD (spray chamber 10 deg.C, drift tube 80 deg.C) 6 uL (6 ug, water) 10

260 nm 6 uL (6 ug, water) 0 0 5 10 15 min

Unison UK-C18, 150 x 4.6 mm A: 50mM ammonium formate, B: acetonitrile 0-20 %B (0-15min) 1 mL/min (10MPa), 37 deg.C

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI593E-JC15 North America Other Countries No.TI617E

Coumarins

1 CH2OH 5 8 O O 6 OH HO OH 3 O O 2 4 HO 1 7 0-40%B esculin (0-30min) 2 HO 5 3 6 8 2 HO O O 1 4 7 0-50%B esculetin (0-50min) 5 3 3 6 8 2 4 HO O O 1 7 0-50%B 7-hydroxycoumarin (0-50min)

mAU 5 6 8 4 H3CO 3 200 1 2 4 O O 7 0-60%B HO (0-50min) scopoletin 6 8 3,4 5 5 OH 2 1 7 0-60%B (0-50min) O O 8 4-hydroxycoumarin 100 3 5 6 2 1 4 6 7 0-60%B (0-50min) O O 6 5 8 coumarin 2 3 1 4 7 0-60%B 7 (0-50min) 0 O O 3,4-dihydrocoumarin 0 10 20 30 min 8 O 150 x 4.6 mm ONa CH2 C CH3 A: water / acetic acid = 100 / 1 B: acetonitrile / acetic acid = 100 / 1 O O 1 mL/min (9-11MPa), 37 deg.C, 270 nm warfarin 2 uL (0.2-1.2 ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI617E-JI09 North America Other Countries No.TI621E

Plerixafor (Chemokine receptor antagonist)

H H N N

HN N N NH

N N H plerixafor H 1 mAU

100

0 2 4 6 8 min

Unison UK-C18, 150 x 4.6 mm 20mM sodium heptanesulfonate in 20mM H3PO4 / acetonitrile = 65 / 35 1 mL/min (10MPa), 37 deg.C, 220 nm, 2 uL (2 ug, water)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI621E-JG21 North America Other Countries No.TI628E

Coumarins 1 CH2OH O O A: water /acetic acid OH HO 5 = 100 /0.1 OH B: acetonitrile /acetic acid HO O O = 100 /0.1 esculin 3 2 HO 2 8 4 6 1 7 HO O O esculetin

3 HO O O 5 8 6 7-hydroxycoumarin 2 mAU H3CO 3 A: water /acetic acid 4 = 100 /0.5 4 HO O O 1 B: acetonitrile /acetic acid 100 7 = 100 /0.5 scopoletin

5 O O coumarin 6 5 8 6 OH 50 A: water /acetic acid 2 3 = 100 /1 O O B: acetonitrile /acetic acid 4-hydroxycoumarin 4 = 100 /1 1 7 7 O O 0 3,4-dihydrocoumarin

0 10 20 30 min 8 O ONa CH2 C CH3 Scherzo SM-C18, 150 x 4.6 mm 0-60 %B (0-30min) 1 mL/min (9MPa), 37 deg.C, 270 nm O O warfarin 2 uL (0.2-1.2 ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI628E-JJ15 North America Other Countries No.TI639E

Cold medicine compounds

1 N CH3 2 N 3 H3C O CH2CH2 N C CH HO COCH2CH2CH3 H 3

Cl H3C O propylparaben dl-chlorpheniramine dextromethorphan 3

1 2 Unison UK-Phenyl, 150 x 4.6 mm 100mM ammonium formate / acetonitrile = 80 / 20 1 mL/min (9MPa), 37 deg.C, 235 nm, 2 uL (0.4-1.8 ug) 2 3 1 Unison UK-C8, 150 x 4.6 mm 100mM ammonium formate / methanol = 60 / 40 1 mL/min (16MPa), 37 deg.C, 235 nm, 2 uL (0.4-1.8 ug) 2 3 1 Cadenza CW-C18, 150 x 4.6 mm 100mM ammonium formate / methanol = 60 / 40 mAU 1 mL/min (17MPa), 37 deg.C, 235 nm, 40 2 uL (0.4-1.8 ug) 3 2 1 Unison UK-C18, 150 x 4.6 mm 100mM ammonium formate / methanol = 50 / 50 1 mL/min (16MPa), 37 deg.C, 235 nm, 2 uL (0.4-1.8 ug) 2 3 1 Cadenza CD-C18, 150 x 4.6 mm 100mM ammonium formate / methanol = 50 / 50 1 mL/min (17MPa), 37 deg.C, 235 nm, 0 2 uL (0.4-1.8 ug) 0 5 10 15 min

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI639E-KB02 North America Other Countries No.TI640E

Cold medicine compounds

CH3 O 1 N CH3 2 N 3 CH2CH2 N HO COCH2CH2CH3 C CH H 3

Cl dl-chlorpheniramine H3C O dextromethorphan propylparaben

2 mAU 100 3

1 A: water / formic acid = 100 / 0.1 B: acetonitrile / formic acid = 100 / 0.5 3 15-80 %B (0-10min) 2 80 %B (10-13min) 15 %B (13-30min) 1 mixer: 600uL 0 0.4 mL/min (8MPa) 37 deg.C, 280 nm 0 5 10 15 min 1 uL (0.2-0.9ug)

1 2 mAU 100

2 1 3

100mM ammonium formate / acetonitrile = 45 / 55 0.4 mL/min (8MPa) 0 37 deg.C, 235nm, 0 5 10 15 min 1 uL (0.2-0.9ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI640E-JL27 North America Other Countries No.TI662E

Penicillin antibiotics

COOH O O N CH3

mAU CH N S 3 H H 40 penicillin G

OCH 3 COOH O O N CH3 penicillin G, 2 mg/mL x 5 uL CH N S 3 H H 20 methicillin, 2 mg/mL x 1 uL OCH3 methicillin ampicillin, 2 mg/mL x 5 uL

COOH amoxicillin, 2 mg/mL x 2 uL O O N CH3 carbenicillin, 10 mg/mL x 5 uL CH N S 3 0 H H NH2 0 5 10 15 min ampicillin

COOH HO O O N CH3 CH S 3

mAU N H H NH2 40 amoxicillin

COOH O O N CH3 CH N S 3 H H penicillin G, 2 mg/mL x 5 uL COOH 20 methicillin, 2 mg/mL x 1 uL carbenicillin ampicillin, 2 mg/mL x 5 uL 75 x 4.6mm A: 5mM ammonium acetate amoxicillin, 2 mg/mL x 2 uL B: 100mM ammonium acetate / carbenicillin, 10 mg/mL x 5 uL acetonitrile = 50 / 50 0 0-70 %B (0-10min) 1.0 mL/min(6-7MPa) 0 5 10 15 min 37 deg.C, 260 nm

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI662E-KD28 North America Other Countries No.TI672E

Basic pharmaceutical compounds

1 HO 2 3 H OH 1 CCH2NHCH3 HCl 4 A: water /HCOOH = 100 /0.5 phenylephrine

mAU B: ACN /HCOOH = 100 /1 300 20-80 %B (0-15 min)

O 3 CH2CH3 C NHCH2H3CN CH2CH3 4 1 2 HCl 2 A: water /HCOOH = 100 /0.1 HN C CH3 B: 100 mM HCOONH O 200 4 /ACN = 50 /50 N-acetylprocainamide 0-100 %B (0-15 min)

O CH2CH3 C OCH2CH2N CH2CH3 3 3 HCl

1 100 4 NH2 procaine 2 A: 10 mM HCOONH4 B: 100mM HCOONH4 /ACN = 50 /50 0-100 %B (0-15 min) N 4 HCl N CH2

0 naphazoline 0 5 10 15 min

Scherzo SW-C18, 150 x 3 mm 0.4 mL/min (9 MPa), 37 deg.C, 260 nm, 2 uL (0.05-3.2 ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI672E-KG07 North America Other Countries No.TI676E

HT Ultra-high throughput LC-MS/MS analysis of drugs in blood plasma

HT s t n u o c

, a e r A

Cadenza CD-C18 HT, 50 x 2 mm A: 0.1% HCOOH in water, B: 0.1% HCOOH in acetonitrile 2µL (20µL plasma + 500µL acetonitrile) Shimadzu UFLC - AB Sciex API5000 (ESI positive, MRM) NFD(nifedipine) 347 > 254, WAR(warfarin) 309 >163, DCL(diclofenac) 296 > 214, CBP(2-amino-5-chlorobenzophenone) 232 > 126 Courtesy of Dr. IKEHARA Tatsuya, Shionogi Co., Ltd., JAPAN Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI676E-KG16 North America Other Countries No.TI678E

Acetaminophen and metabolite

2 1 2 H O N CCH3 HO N CCH3 O 1 O N-acetyl-4-benzoquinone acetaminophen imine

1 2 mAU

1 2 400

1 2

200

2 1

0 0 5 10 min

150 x 3 mm A: 2mM ammonium acetate B: 100mM ammonium acetate / acetonitrile = 50 / 50 0-20 %B (0-10min) 0.5 mL/min (9-11MPa), 37 deg.C, 260 nm, 1 uL (0.8 ug)

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI678E-KH05 North America Other Countries No.TI679E

Acetaminophen and metabolite

1 2 H O N CCH3 1 HO N CCH3 O O N-acetyl-4-benzoquinone 2 acetaminophen imine

1 2 mAU

400 1 2

2 1

200

2 1

0 0 5 10 min

150 x 3 mm water / acetonitrile / formic acid = 95 / 5 / 0.1 0.5 mL/min (10-11MPa), 37 deg.C, 260 nm, 1 uL (0.8 ug)

AUTHORIZED DISTRIBUTOR MZ-Analysentechnik GmbH, Barcelona-Allee 17• D-55129 Mainz Tel +49 6131 880 96-0, Fax +49 6131 880 96-20 e-mail: [email protected], www.mz-at.de

Imtakt USA ([email protected]) Imtakt Corp./JAPAN ([email protected]) TI679E-KH05 North America Other Countries