Analysis of betamethasone, dexamethasone and related compounds by liquid chromatography/electrospray mass spectrometry

被引：68

作者：

Arthur, KE ^{[1
]}

Wolff, JC ^{[1
]}

Carrier, DJ ^{[1
]}

机构：

[1] GlaxoSmithKline Pharmaceut, Med Res Ctr, Stevenage SG1 2NY, Herts, England

来源：

RAPID COMMUNICATIONS IN MASS SPECTROMETRY | 2004年 / 18卷 / 06期

关键词：

D O I：

10.1002/rcm.1386

中图分类号：

Q5 [生物化学];

学科分类号：

071010 ; 081704 ;

摘要：

A reversed-phase high-performance liquid chromatography/electrospray ionisation mass spectrometry (HPLC/ESI-MS) method has been developed to conclusively differentiate the epimers betamethasone and dexamethasone and various esterification products (betamethasone and dexamethasone 21-acetate, betamethasone and dexamethasone 21-phosphate, betamethasone 17-valerate, betamethasone 21-valerate and betamethasone 17,21-dipropionate) in counterfeit drugs. Good separation with baseline resolution of all epimers or isomers was obtained on a Zorbax Eclipse XDB or Luna C8 column, using a step gradient with mobile phases of 0.05 M ammonium acetate and acetonitrile. Betamethasones can also be distinguished by the relative abundance of their m/z 279 ion in the positive electrospray tandem mass spectra. The LC/MS or LC/MS/MS method developed was successfully applied to the analysis of drug product samples, i.e. creams and tablets. Copyright (C) 2004 John Wiley Sons, Ltd.

引用

页码：678 / 684

页数：7

共 17 条

[1]

Antignac JP, 2000, RAPID COMMUN MASS SP, V14, P33, DOI 10.1002/(SICI)1097-0231(20000115)14:1<33::AID-RCM829>3.3.CO

[2]

2-I

[3] Analysis of corticosteroids in hair by Liquid chromatography-electrospray ionization mass spectrometry [J].

Bévalot, F ;

Gaillard, Y ;

Lhermitte, MA ;

Pépin, G .

JOURNAL OF CHROMATOGRAPHY B, 2000, 740 (02) :227-236

[4] STEREOCHEMICAL ANALYSIS OF BETAMETHASONE AND DEXAMETHASONE BY DERIVATIZATION AND HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY [J].

CHEN, SH ;

WU, SM ;

WU, HL .

JOURNAL OF CHROMATOGRAPHY, 1992, 595 (1-2) :203-208

[5] Identification of ten corticosteroids in human hair by liquid chromatography-ionspray mass spectrometry [J].

Cirimele, V ;

Kintz, P ;

Dumestre, V ;

Goullé, JP ;

Ludes, B .

FORENSIC SCIENCE INTERNATIONAL, 2000, 107 (1-3) :381-388

[6] Differentiation between dexamethasone and betamethasone in a mixture using multiple mass spectrometry [J].

De Wasch, K ;

De Brabander, HF ;

Van de Wiele, M ;

Vercammen, J ;

Courtheyn, D ;

Impens, S .

JOURNAL OF CHROMATOGRAPHY A, 2001, 926 (01) :79-86

[7] Validation of a screening method for corticosteroids in doping analysis by liquid chromatography/tandem mass spectrometry [J].

Deventer, K ;

Delbeke, FT .

RAPID COMMUNICATIONS IN MASS SPECTROMETRY, 2003, 17 (18) :2107-2114

[8] Identification of main corticosteroids as illegal feed additives in milk replacers by liquid chromatography atmospheric pressure chemical ionisation mass spectrometry [J].

Fiori, M ;

Pierdominici, E ;

Longo, F ;

Brambilla, G .

JOURNAL OF CHROMATOGRAPHY A, 1998, 807 (02) :219-227

[9] Method for confirmation of synthetic corticosteroids in doping urine samples by liquid chromatography-electrospray ionisation mass spectrometry [J].

Fluri, K ;

Rivier, L ;

Dienes-Nagy, A ;

You, CH ;

Maître, A ;

Schweizer, C ;

Saugy, M ;

Mangin, P .

JOURNAL OF CHROMATOGRAPHY A, 2001, 926 (01) :87-95

[10] Sensitive liquid chromatographic/tandem mass spectrometric method for the determination of beclomethasone dipropionate and its metabolites in equine plasma and urine [J].

Guan, FY ;

Uboh, C ;

Soma, L ;

Hess, A ;

Luo, Y ;

Tsang, DS .

JOURNAL OF MASS SPECTROMETRY, 2003, 38 (08) :823-838

← 1 2 →