Simultaneous measurement of urinary bisphenol A and alkylphenols by automated solid-phase extractive derivatization gas chromatography/mass spectrometry
Simultaneous measurement of urinary bisphenol A and alkylphenols by automated solid-phase extractive derivatization gas chromatography/mass spectrometry
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DOI：
10.1021/ac0303158
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发表时间：
2003-12-15
影响因子：
7.4
通讯作者：
Calafat, AM
中科院分区：
文献类型：
--
作者：
Kuklenyik, Z;Ekong, J;Calafat, AM
双酚A （BPA）和烷基酚（APs）是广泛使用的工业化学品。BPA用于制造聚碳酸酯塑料和环氧树脂；APs用于制造烷基酚聚氧乙烯酯，这是一种常见的非离子表面活性剂。在工业生产过程中，聚碳酸酯塑料和非离子表面活性剂降解后，BPA和APs会渗入环境。环境暴露于这些酚类化合物与野生动物的不利生殖和发育影响有关。我们开发了一种灵敏且可靠的方法来测量BPA和六种ap；尿中的3-叔丁基酚、4-叔丁基酚、4-正辛基酚、4-叔辛基酚、4-正壬基酚和技术级壬基酚。该方法是基于使用自动固相萃取（SPE）耦合同位素稀释-气相色谱/质谱（GC/MS）。在自动化固相萃取过程中，苯酚从尿液基质中提取，并在市售的苯乙烯-二乙烯基苯共聚物基固相萃取筒上使用五氟溴衍生化。经固相萃取柱洗脱后，用GC/MS分析固相萃取液中衍生酚类物质。该方法在加标池尿液样本和暴露者尿液样本上进行了验证，其检出限与1 mL尿液中0.1 ng相似。
Bisphenol A (BPA) and alkylphenols (APs) are widely used industrial chemicals. BPA is used to manufacture polycarbonate plastic and epoxy resins; APs are used to make alkylphenol ethoxylates, common nonionic surfactants. BPA and APs can leach into the environment during industrial production and after degradation of the polycarbonate plastics and nonionic surfactants. Environmental exposure to these phenolic compounds has been associated with adverse reproductive and developmental effects in wildlife. We developed a sensitive and robust method for measuring BPA and six APs; 3-tert-butylphenol, 4-tert-butylphenol, 4-n-octylphenol, 4-tert-octylphenol, 4-n-nonylphenol, and technical-grade nonylphenol in urine. The method is based on the use of automated solid-phase extraction (SPE) coupled to isotope dilution-gas chromatography/mass spectrometry (GC/MS). During the automated SPE process, the phenols are both extracted from the urine matrix and derivatized, using pentafluorobenzyl bromide, on commercially available styrene-divinylbenzene copolymer-based SPE cartridges. After elution from the SPE column, the derivatized phenols in the SPE eluate are analyzed by GC/MS. The method, validated on spiked pooled urine samples and on urine samples from exposed persons, has limits of detection of similar to0.1 ng in 1 mL of urine.