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Derivatization procedures for the detection of estrogenic chemicals by gas chromatography/mass spectrometry
Author(s) -
Ding WangHsien,
Chiang ChengChe
Publication year - 2002
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.819
Subject(s) - chemistry , derivatization , chromatography , mass spectrometry , gas chromatography–mass spectrometry , estriol , gas chromatography , selected ion monitoring , silylation , yield (engineering) , detection limit , organic chemistry , biochemistry , materials science , hormone , metallurgy , catalysis
Abstract This work evaluated derivatization procedures for detecting both natural and synthetic estrogenic chemicals by gas chromatography/mass spectrometry (GC/MS). Different silylating agents, mainly trimethylsilylating (TMS) agents, were compared, and the roles of various content of trimethylchlorosilane (TMCS, as a stimulator) were investigated. The difference in the abundances of the derivatives was caused by the steric hindrance of multiple hydroxyl groups and ethynyl groups in the structures of estrogenic chemicals. The use of TMCS produces an increase in the derivatization yield, especially for the compounds with multiple hydroxyl groups (i.e., 17β‐estradiol (E 2 ) and estriol (E 3 )). Mass spectra of O‐TMS derivatives and tentative fragmentation profiles are proposed. Molecular ions were the base peaks for all the derivatives, and were used as the quantitation ions to obtain maximum detection sensitivity and specificity. Sample enrichment was achieved by Oasis® HLB solid‐phase extraction cartridges. The quantitation limits of these compounds ranged from 5 to 10 ng/L in 1000‐mL water samples. Recovery of the estrogenic chemicals in spiked various water samples ranged from 78 to 102% while relative standard deviation (RSD) ranged from 1 to 15%. Copyright © 2002 John Wiley & Sons, Ltd.