Stir bar sorptive extraction with in situ derivatization and thermal desorption–gas chromatography–mass spectrometry in the multi-shot mode for determination of estrogens in river water sa

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• 作者：Kawaguchi ; Migaku ; Ishii ; Yumiko ; Sakui ; Norihiro ; Okanouchi ; Noriya ; Ito ; Rie ; Inoue ; Koichi ; et. al.
• 关键词：Estrogens ; Stir bar sorptive extraction ; Derivatization ; GC ; Water analysis ; Thermal desorption
• 刊名：Journal of Chromatography A
• 出版年：2004
• 期刊代码：47_00219673
• 类别：ch
• 出版时间：September 17, 2004
• 卷：1049
• 期：1-2
• 页码：1-8
• 文件大小：209 K

摘要

A novel method for the trace analysis of natural and synthetics estrogens, such as estrone (E1), 17β-estradiol (E2) and 17α-ethynylestradiol (EE), in river water sample was developed, which involved stir bar sorptive extraction (SBSE) with in situ derivatization followed by thermal desorption (TD)&ndash;gas chromatography&ndash;mass spectrometry (GC&ndash;MS). The derivatization conditions with acetic acid anhydride and the SBSE conditions such as sample volume and extraction time were investigated. In addition, the single and multi-shot modes in TD were investigated. The detection limits of E1, E2 and EE in river water sample were 0.2, 0.5 and 1pgml⁻¹ (ppt), respectively, in the multi-shot mode using five stir bars. The calibration curves for E1, E2 and EE were linear and had correlation coefficients >0.99. The average recoveries of E1, E2 and EE from all sample volumes were higher than 90%(R.S.D. < 10%) with correction using an added surrogate standard such as estrone-¹³C₄, 17β-estradiol-¹³C₄ or 17α-ethynylestradiol-¹³C₄. This simple, accurate, sensitive and selective analytical method may be applicable to the determination of trace amounts of estrogens in water samples.