Trace analysis of phenolic xenoestrogens in water samples by stir bar sorptive extraction with in situ derivatization and thermal desorption-gas chromatography-mass spectrometry.
Trace analysis of phenolic xenoestrogens in water samples by stir bar sorptive extraction with in situ derivatization and thermal desorption-gas chromatography-mass spectrometry.
复制标题
DOI：
10.1016/j.chroma.2004.04.044
复制
发表时间：
2004-07
期刊：
影响因子：
--
通讯作者：
Migaku Kawaguchi;K. Inoue;M. Yoshimura;N. Sakui;N. Okanouchi;R. Ito;Y. Yoshimura;H. Nakazawa
中科院分区：
文献类型：
--
作者：
Migaku Kawaguchi;K. Inoue;M. Yoshimura;N. Sakui;N. Okanouchi;R. Ito;Y. Yoshimura;H. Nakazawa
建立了一种采用搅拌棒吸附萃取 (SBSE) 原位同时测定水样中痕量酚类异雌激素的方法，例如 2,4-二氯苯酚 (2,4-DCP)、4-叔丁基苯酚 (BP)、4-叔辛基苯酚 (OP)、4-壬基苯酚 (NP)、五氯苯酚 (PCP) 和双酚 A (BPA)。衍生化，然后进行热解吸（TD）-气相色谱-质谱（GC-MS）分析。研究了乙酸酐衍生化的条件。将聚二甲基硅氧烷 (PDMS) 涂层的搅拌棒和衍生剂添加到 10ml 水样中，并在顶空瓶中于室温 (25°C) 下开始搅拌 10-180 分钟。然后，通过 TD-GC-MS 分析提取物。原位衍生化SBSE的最佳时间为90分钟。 2,4-DCP、BP、OP、NP、PCP 和 BPA 的检测限分别为 2、1、0.5、5、2 和 2pgml−1。该方法对2,4-DCP、BP、OP、NP、PCP和BPA分别在10、5、2、20、10和10-1000pgml−1浓度范围内表现出良好的线性关系，相关系数均高于0.99。使用添加的替代标准品进行校正后，河水样品中这些化合物的平均回收率等于或高于 93.9%（R.S.D. <7.2%）。该方法简单、准确、灵敏、选择性强，可用于河水样品中微量酚类异雌激素的测定。
A method for the simultaneous measurement of trace amounts of phenolic xenoestrogens, such as 2,4-dichlorophenol (2,4-DCP), 4-tert-butylphenol (BP), 4-tert-octylphenol (OP), 4-nonylphenol (NP), pentachlorophenol (PCP) and bisphenol A (BPA), in water samples was developed using stir bar sorptive extraction (SBSE) with in situ derivatization followed by thermal desorption (TD)–gas chromatography–mass spectrometry (GC–MS) analysis. The conditions for derivatization with acetic acid anhydride were investigated. A polydimethylsiloxane (PDMS)-coated stir bar and derivatization reagents were added to 10ml of water sample and stirring was commenced for 10–180min at room temperature (25°C) in a headspace vial. Then, the extract was analyzed by TD–GC–MS. The optimum time for SBSE with in situ derivatization was 90min. The detection limits of 2,4-DCP, BP, OP, NP, PCP and BPA were 2, 1, 0.5, 5, 2 and 2pgml−1, respectively. The method showed good linearity over the concentration ranges of 10, 5, 2, 20, 10 and 10–1000pgml−1for 2,4-DCP, BP, OP, NP, PCP and BPA, respectively, and the correlation coefficients were higher than 0.99. The average recoveries of those compounds in river water samples were equal to or higher than 93.9% (R.S.D. <7.2%) with correction using the added surrogate standards. This simple, accurate, sensitive and selective method can be used in the determination of trace amounts of phenolic xenoestrogens in river water samples.