以固相萃取法及氣相層析質譜儀對水環境中動情激素類有機污染物之分析與研究; Analysis of estrogens in environmental water samples using solid-phase extraction and gas chromatography–mass spectrometry

Please use this identifier to cite or link to this item: http://ir.lib.ncu.edu.tw/handle/987654321/5890

Title:	以固相萃取法及氣相層析質譜儀對水環境中動情激素類有機污染物之分析與研究;Analysis of estrogens in environmental water samples using solid-phase extraction and gas chromatography–mass spectrometry
Authors:	江政哲;Cheng-Che Chiang
Contributors:	化學研究所
Keywords:	水環境;衍生化;氣相層析質譜儀;動情激素;estrogen;gas chromatography mass spectrometry;derivatization
Date:	2002-06-18
Issue Date:	2009-09-22 10:09:40 (UTC+8)
Publisher:	國立中央大學圖書館
Abstract:	本研究藉著矽烷化衍生法將天然以及人工合成的動情激素類化合物衍生為低極性高揮發度的衍生物，同時搭配具有高靈敏度和良好分離效果的氣相層析質譜儀來對環境水樣作一分析。衍生化過程中藉著添加不同比例的催化劑(TMCS)至衍生試劑中(BSTFA)，來探討不同配方衍生試劑對最終衍生物的影響。實驗發現除了部分分析物無法完全衍生的主要因素是因為相鄰的OH官能基與乙炔基帶來的立體障礙影響，而隨著催化劑比例的增加也可以使具有2~3個OH官能基的分析物(例如：estriol , E3 ; 17α-ethynylestradiol , EE2)增加完全衍生的比例。在O-TMS衍生物的質譜圖中也發現，所有O-TMS的衍生物其強度最高的離子基峰皆為分子離子，因此為了求得在定性定量上最高的靈敏度，離子選擇主要皆以分子離子為主，另外部分碎裂較嚴重的衍生物，則再加上相對強度次高的特徵斷裂離子以加強積分訊號。萃取部分則是採用全新研發的Oasis® HLB固相萃取管柱，經由去離子水與真實水樣基質干擾的驗證下，回收率皆可以達到80﹪以上，而目前所抽查的四條台灣河流當中，由其分析結果得知目前台灣河流當中，天然與人工合成的動情激素類化合物含量皆低於本方法之偵測極限5 ppt。 This work evaluated derivatization procedures for detecting both natural and synthetic estrogenic chemicals to obtain derivatives with high selectivity for using in gas chromatography-mass spectrometry (GC/MS) analysis of environmental samples. Different silylating agents, mainly trimethylsilylating agents (TMS), 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 sterical hindrance of multiple hydroxyl groups and ethynyl group 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., estriol (E3) and 17a-ethynylestradiol (EE2)). Mass spectra of O-TMS-derivatives and tentative fragmentation profiles are also displayed. Molecular ions were the base peaks in all the derivatives, and were used as the quantitation ions to obtain maximum detection sensitivity and specificity. Sample enrichment was achieved by newly developed Oasisâ HLB solid-phase extraction cartridges. Recovery of the estrogenic chemicals in spiked various water samples ranged from 78% to 102% while RSD ranged from 1 to 15%.
Appears in Collections:	[Graduate Institute of Chemistry] Electronic Thesis & Dissertation

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