Capillary gas chromatography of acidic non-steroidal antiinflammatory drugs as tert.-butyldimethylsilyl derivatives

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)tr...

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Published in:Journal of Chromatography A 1993-07, Vol.641 (2), p.319-327
Main Authors: Kim, Kyoung-Rae, Shim, Wean-Hee, Shin, You-Jin, Park, Jongsei, Myung, Seoungwon, Hong, Jongki
Format: Article
Language:English
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Summary: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 μg with high overall precisions. The method provided simultaneous screening and accurate confirmation of each drug when applied to serum samples spiked with NSAIDS.
ISSN:0021-9673
DOI:10.1016/0021-9673(93)80148-2