New Discoveries of Heating Effect on Trimethylsilyl Derivatization for Simultaneous Determination of Steroid Endocrine Disrupting Chemicals by GC¨CMS

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• 作者：Bin Huang ; Xuejun Pan ; Jingliang Liu ; Kai Fang ; Yu Wang and Jianpei Gao
• 关键词：Gas chromatography– ; mass spectrometry ; Endocrine disrupting chemicals ; Steroids ; N ; O ; Bis(trimethylsilyl)trifluoroacetamide ; N ; Methyl ; N ; (trimethylsilyl)trifluoroacetamide
• 刊名：Chromatographia
• 出版年：2010
• 出版时间：January, 2010
• 年：2010
• 卷：71
• 期：1-2
• 页码：149-153
• 全文大小：328.3 KB

文摘

Most previously described derivatization procedures with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) or N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) for the GC–MS analysis of steroids, such as estrone (E1), 17β-estradiol (E2), estriol (E3) and 17α-ethynylestradoil (EE2), used a heating process of 45–80 ¡ãC (typically 70 ¡ãC) for 25–60 min, usually in combination with a catalyst. However, we found that it is not necessary to heat and add catalyst for the derivatization with BSTFA. Best reaction conditions for MSTFA are heating at 70 ¡ãC for 10 min. Derivatization of EE2 using MSTFA without heating results in three products: TMS-E1, mono-TMS-EE2 and di-TMS-EE2.