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 samples.
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 samples.
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DOI：
10.1016/s0021-9673(04)01341-x
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发表时间：
2004-09
期刊：
影响因子：
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通讯作者：
Migaku Kawaguchi;Y. Ishii;N. Sakui;N. Okanouchi;R. Ito;K. Inoue;Koichi Saito;H. Nakazawa
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文献类型：
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作者：
Migaku Kawaguchi;Y. Ishii;N. Sakui;N. Okanouchi;R. Ito;K. Inoue;Koichi Saito;H. Nakazawa
采用搅拌棒吸附萃取(SBSE) -原位衍生-热脱附(TD) -气相色谱-质谱联用（GC-MS）的方法，对河流水样中天然和合成雌激素雌酮（E1）、17β-雌二醇（E2）和17α-乙基雌二醇（EE）进行了痕量分析。考察了乙酸酐衍生化条件和萃取时间等SBSE条件。此外，还研究了TD的单发和多发模式。在5根搅拌棒的多枪模式下，河流水样中E1、E2和EE的检出限分别为0.2、0.5和1pgml−1（ppt）。E1、E2和EE的标度曲线呈线性关系，相关系数为>0.99。在添加雌酮- 13c4、17β-雌二醇- 13c4或17α-乙基雌二醇- 13c4等替代标准品进行校正后，E1、E2和EE的平均回收率均大于90% （rsd < 10%）。该方法简便、准确、灵敏、选择性好，可用于水样中微量雌激素的测定。
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)–gas chromatography–mass spectrometry (GC–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-13C4or 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.