ON HPLC COLUMNS Pharmaceutical Compounds Cosmetics 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 50 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 50 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 50 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 2 1 nilvadipine 1 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 O 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 0 O HO 0 5 10 15 20 25 min 4 H3CO 2-hydroxyestrone 3-methyl ether O 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 10 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 O CCH3 3 H3C OH CH3 H H H O 17 a -hydroxyprogesterone O 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.