Analytical method for urinary metabolites as biomarkers for monitoring exposure to phthalates by gas chromatography/mass spectrometry
Analytical method for urinary metabolites as biomarkers for monitoring exposure to phthalates by gas chromatography/mass spectrometry
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尿代谢物作为生物标志物的分析方法，用于通过气相色谱/质谱法监测邻苯二甲酸盐暴露
DOI：
10.1002/bmc.3910
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发表时间：
2017
影响因子：
1.8
通讯作者：
Toshiaki Yoshida
中科院分区：
文献类型：
--
作者：
Fujita Misuzu;Sato Yasunori;Nagashima Kengo;Takahashi Sho;Hata Akira;Toshiaki Yoshida
邻苯二甲酸酯，广泛用作增塑剂，已在室内空气中检测到，但很少有关于分析尿液代谢物作为生物标志物以监测邻苯二甲酸二正戊酯或邻苯二甲酸二正己酯暴露的方法的报告。本文介绍了一种用于测定含有这两种化合物的邻苯二甲酸酯尿液代谢物的具有成本效益且灵敏的分析方法。对9种尿邻苯二甲酸酯代谢产物进行酶水解，并使用甲苯进行提取：邻苯二甲酸单甲酯、邻苯二甲酸单乙酯、邻苯二甲酸单异丁酯、邻苯二甲酸单正丁酯、邻苯二甲酸单正戊酯、邻苯二甲酸单正己酯、邻苯二甲酸单环己烷酯、邻苯二甲酸单苄酯和邻苯二甲酸单（2-乙基-5-羧基戊基）酯。转化为叔丁基二甲基甲硅烷基衍生物后，通过气相色谱/质谱法在电子轰击电离模式下对其进行分析。代谢物的校准曲线在尿液浓度高达30 μ g/L时呈线性，表明它们可以准确和精确地测定（检测限0.1 - 0.4 μ g/L，定量限0.3 - 1.3 μ g/L）。收集的尿样可在− 20 ° C下储存长达1个月。拟定的分析方法用于检查7名健康志愿者的尿样。这种方法应该是有用的监测邻苯二甲酸酯在一般人群中的暴露。
Phthalates, widely used as plasticizers, have been detected in indoor air, but there have been few reports on methods of analyzing urinary metabolites as biomarkers to monitor exposure to di‐n‐pentyl phthalate or di‐n‐hexyl phthalate. Presented here is a cost‐effective and sensitive analytical method for the determination of urinary metabolites of phthalates containing these two compounds. Nine urinary phthalate metabolites were enzymatically hydrolyzed and extracted with toluene: monomethyl phthalate, monoethyl phthalate, monoisobutyl phthalate, mono‐n‐butyl phthalate, mono‐n‐pentyl phthalate, mono‐n‐hexyl phthalate, monocyclohexyl phthalate, monobenzyl phthalate and mono(2‐ethyl‐5‐carboxypentyl) phthalate. After transformation to theirtert‐butyldimethylsilyl derivatives, they were analyzed by gas chromatography/mass spectrometry in the electron impact ionization mode. The calibration curves for the metabolites were linear at urinary concentrations of up to 30 μg/L, showing that they could be determined accurately and precisely (detection limits 0.1–0.4 μg/L, quantification limits 0.3–1.3 μg/L). The urine samples collected could be stored for up to 1 month at −20°C. The proposed analytical method was used to examine urine samples from seven healthy volunteers. This method should be useful for monitoring phthalate exposure in the general population.