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

作者：Huang, Bin; Pan, Xuejun^*; Liu, Jingliang; Fang, Kai; Wang, Yu; Gao, Jianpei

来源：Chromatographia, 2010, 71(1-2): 149-153.

DOI：10.1365/s10337-009-1392-5

• Gas chromatography-mass spectrometry
• Endocrine disrupting chemicals
• Steroids
• N,O-Bis(trimethylsilyl)trifluoroacetamide
• N-Methyl-N-(trimethylsilyl)trifluoroacetamide

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), 17 beta-estradiol (E2), estriol (E3) and 17 alpha-ethynylestradoil (EE2), used a heating process of 45-80 A degrees C (typically 70 A degrees C) 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 A degrees C for 10 min. Derivatization of EE2 using MSTFA without heating results in three products: TMS-E1, mono-TMS-EE2 and di-TMS-EE2.

• 出版日期2010-1
• 单位昆明理工大学