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Simultaneous determination of multiple phthalate metabolites and bisphenol-A in human urine by liquid chromatography-tandem mass spectrometry

机译:液相色谱 - 串联质谱法同时测定人尿中的多邻苯二甲酸代谢物和双酚-A

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摘要

Phthalates and bisphenol A are environmental endocrine-disrupting chemicals used widely in common consumer products. There is increasing concern about human exposure to phthalates and bisphenol A due to the potential adverse effects related to the anti-androgenic activity of phthalates and estrogenic activity of bisphenol A. In assessing environmental exposure to phthalates and bisphenol A, it is essential to have a validated analytical method that can quantify trace concentrations of phthalate metabolites and bisphenol A in humans. In this study, we developed and validated an accurate, sensitive, and robust LC-MS/MS method to simultaneously quantify 5 phthalate monoester metabolites, including mono-methyl phthalate, mono-ethyl phthalate, mono-butyl phthalate, mono-benzyl phthalate, mono-2-ethylhexyl phthalate, and bisphenol A in human urine. In this method, the phthalate metabolites and bisphenol A, along with their isotope labeled internal standards, were extracted from 200 μl of human urine using automated off-line solid phase extraction. The analytes were quantitatively determined using LC-MS/MS operated in negative electrospray ionization multiple reaction-monitoring mode. The limit of quantification was 0.3 ng/ml for mono-methyl phthalate, mono-ethyl phthalate, mono-benzyl phthalate and bisphenol A, and 1 ng/ml for mono-butyl phthalate and mono-2-ethylhexyl phthalate. The precision and accuracy were well within the acceptable 15% range. This validated method has been used successfully in assessing exposure to phthalates and bisphenol A in humans.
机译:邻苯二甲酸盐和双酚A是破坏环境内分泌的化学物质,广泛用于普通消费品中。由于与邻苯二甲酸酯的抗雄激素活性和双酚A的雌激素活性相关的潜在不利影响,人们对邻苯二甲酸酯和双酚A的暴露日益引起关注。在评估环境对邻苯二甲酸酯和双酚A的暴露时,必不可少的是经过验证的分析方法,可以定量分析人体中邻苯二甲酸酯代谢物和双酚A的痕量浓度。在这项研究中,我们开发并验证了一种准确,灵敏且稳健的LC-MS / MS方法,可同时定量5种邻苯二甲酸酯单酯代谢物,包括邻苯二甲酸单甲酯,邻苯二甲酸单乙酯,邻苯二甲酸单丁酯,邻苯二甲酸单苄酯,人尿中的邻苯二甲酸单-2-乙基己酯和双酚A。在这种方法中,使用自动离线固相萃取从200μl人尿中萃取了邻苯二甲酸酯代谢物和双酚A及其同位素标记的内标。使用以负电喷雾电离多反应监测模式运行的LC-MS / MS定量测定分析物。邻苯二甲酸单甲酯,邻苯二甲酸单乙酯,邻苯二甲酸单苄酯和双酚A的定量限为0.3 ng / ml,邻苯二甲酸单丁酯和邻苯二甲酸单-2-乙基己酯的定量限为1 ng / ml。精度和准确度均在可接受的15%范围内。该经过验证的方法已成功用于评估人体对邻苯二甲酸酯和双酚A的暴露。

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