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采用 SPE 和 HPLC-MS/MS 法测定双酚 A、双酚 Aß-D-葡糖苷酸、染料木黄酮和染料木黄酮 4'-ß-D-葡糖苷酸。

Measurement of bisphenol A, bisphenol A ß-D-glucuronide, genistein, and genistein 4'-ß-D-glucuronide via SPE and HPLC-MS/MS.

机构信息

Environmental and Occupational Health Sciences Institute, A Joint Institute of Rutgers University and the University of Medicine and Dentistry of New Jersey (UMDNJ), Piscataway, NJ 08854, USA.

出版信息

Anal Bioanal Chem. 2011 Aug;401(3):995-1002. doi: 10.1007/s00216-011-5151-8. Epub 2011 Jun 13.

DOI:10.1007/s00216-011-5151-8
PMID:21667348
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC4376255/
Abstract

Bisphenol A (BPA) is a synthetic industrial reactant used in the production of polycarbonate plastics, and genistein is a natural phytoestrogen abundant in the soybean. Current studies investigating the endocrine-disrupting effects of concomitant exposures to BPA and genistein have warranted the development of an analytical method for the simultaneous measurement of BPA and genistein, as well as their primary metabolites, bisphenol A ß-D-glucuronide (BPA gluc) and genistein 4'-ß-D-glucuronide (genistein gluc), respectively. All four analytes were extracted from rat plasma via solid phase extraction (SPE). Three SPE cartridges and four elution schemes were tested. Plasma extraction using Bond Elut Plexa cartridges with sequential addition of ethyl acetate, methanol, and acetonitrile yielded optimal average recoveries of 98.1 ± 1.8% BPA, 94.9 ± 8.0% genistein, 91.4 ± 6.1% BPA gluc, and 103 ± 6.1% genistein gluc. Identification and quantification of the four analytes were performed by a validated HPLC-MS/MS method using electrospray ionization and selective reaction monitoring. This novel analytical method should be applicable to the measurement of BPA, genistein, BPA gluc, and genistein gluc in urine, cultures, and tissue following in vivo exposures. While reports of the determination of BPA and genistein independently exist, the simultaneous optimized extraction and detection of BPA, genistein, BPA gluc, and genistein gluc have not previously been reported.

摘要

双酚 A(BPA)是一种用于生产聚碳酸酯塑料的合成工业反应物,染料木黄酮是一种富含大豆的天然植物雌激素。目前,研究同时接触 BPA 和染料木黄酮的内分泌干扰作用,有必要开发一种同时测量 BPA 和染料木黄酮及其主要代谢物,即双酚 A β-D-葡糖苷酸(BPA 葡糖苷)和染料木黄酮 4'-β-D-葡糖苷酸(染料木黄酮葡糖苷)的分析方法。所有四种分析物均通过固相萃取(SPE)从大鼠血浆中提取。测试了三种 SPE 小柱和四种洗脱方案。使用 Bond Elut Plexa 小柱,通过依次加入乙酸乙酯、甲醇和乙腈,从血浆中提取,可获得 BPA(98.1±1.8%)、染料木黄酮(94.9±8.0%)、BPA 葡糖苷(91.4±6.1%)和染料木黄酮葡糖苷(103±6.1%)的最佳平均回收率。通过使用电喷雾电离和选择性反应监测的验证高效液相色谱-串联质谱(HPLC-MS/MS)方法对四种分析物进行鉴定和定量。这种新的分析方法应适用于体内暴露后尿液、培养物和组织中 BPA、染料木黄酮、BPA 葡糖苷和染料木黄酮葡糖苷的测量。虽然有关于 BPA 和染料木黄酮单独测定的报道,但以前没有报道过同时优化 BPA、染料木黄酮、BPA 葡糖苷和染料木黄酮葡糖苷的提取和检测。

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