Optimization of silylation using N-methyl-N-(trimethylsilyl)-trifluoroacetamide, N,O-bis-(trimethylsilyl)-trifluoroacetamide and N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide for the determination of the estrogens estrone and 17α-ethinylestradiol by gas chromatography–mass spectrometry
作者： Ali Shareef , Michael J. Angove , John D. Wells
DOI: 10.1016/J.CHROMA.2005.12.098
关键词:
摘要: This paper reports an improved silylation procedure for simultaneous determination of the steroid hormones 17alpha-ethinylestradiol (EE2) and estrone (E1) using gas chromatography-mass spectrometry (GC-MS). follows a re-assessment some popular procedures N-methyl-N-trimethylsilyltrifluoroacetamide (MSTFA), N-O-bis-(trimethylsilyl)-trifluoroacetamide (BSTFA) N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA), which lead to formation trimethylsilyl (TMS) tert-butyldimethylsilyl (TBS) derivatives. Silylation EE2 MSTFA or BSTFA+1% TMCS in ethyl acetate, acetonitrile dichloromethane solvents produced multiple peaks corresponding TMS-E1, 3-mono-TMS-EE2 and/or 3,17-di-TMS-EE2 variable proportions depending on solvent used. When pyridine dimethyl formamide were used under same reaction conditions, only derivative was formed. Derivatization MTBSTFA reagents acetonitrile, dichloromethane, resulted almost 100% conversion mono-TBS-EE2 TBS-E1. Therefore, typical methods previous GC-MS determinations E1 environmental water sediment samples are subject speculation. However, we can confirm that any TMS be with either suitable conditions.
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