CAPILLARY GAS-CHROMATOGRAPHY OF ACIDIC NONSTEROIDAL ANTIINFLAMMATORY DRUGS AS TERT-BUTYLDIMETHYLSILYL DERIVATIVES

被引：16

作者：

KIM, KR ^{[1
]}

SHIM, WH ^{[1
]}

SHIN, YJ ^{[1
]}

PARK, J ^{[1
]}

MYUNG, S ^{[1
]}

HONG, J ^{[1
]}

机构：

[1] KOREA ADV INST SCI & TECHNOL,CTR DOPING CONTROL,SEOUL 131,SOUTH KOREA

来源：

JOURNAL OF CHROMATOGRAPHY | 1993年 / 641卷 / 02期

基金：

新加坡国家研究基金会;

关键词：

D O I：

10.1016/0021-9673(93)80148-2

中图分类号：

O65 [分析化学];

学科分类号：

070302 ; 081704 ;

摘要：

The quantitative conversion of 26 acidic non-steroidal anti-inflammatory drugs (NSAIDs) simultaneously to their corresponding tert.-butyldimethylsilyl (TBDMS) derivatives in a single step was examined. The NSAIDs dissolved in triethylamine were silylated with N-methyl-N-(tert.-butyldimethylsilyl)trifluoroacetamide in isooctane at room temperature for 30 min and subsequently analysed by capillary gas chromatography and gas chromatography-mass spectrometry. The TBDMS derivatives were eluted as untailed sharp peaks and the characteristic [M-57]+ ions in the mass spectra permitted their rapid confirmation. The temperature-programmed retention index (I) sets measured on a DB-5 and DB-17 dual-capillary column system were characteristic of each NSAID to be used for the rapid identification by computer I matching. The derivatization yields of the NSAIDs studied were linear in the range 10-120 mug with high overall precisions. The method provided simultaneous screening and accurate confirmation of each drug when applied to serum samples spiked with NSAIDs.

引用

页码：319 / 327

页数：9

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