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采用气相色谱-质谱法测定人尿中的五种邻苯二甲酸单酯。

Determination of five phthalate monoesters in human urine using gas chromatography-mass spectrometry.

机构信息

Department of Toxicology, Aichi Prefectural Institute of Public Health, 7-6 Nagare, Tsuji-machi, Kita-ku, Nagoya 462-8576, Japan.

出版信息

Bull Environ Contam Toxicol. 2010 Jul;85(1):92-6. doi: 10.1007/s00128-010-0051-8. Epub 2010 Jun 24.

Abstract

We have developed a gas chromatography-mass spectrometry (GC-MS) method to determine five phthalate monoesters (monoethyl phthalate (MEP), mono-n-butyl phthalate (MBP), mono-(2-ethylhexyl) phthalate (MEHP), monoisononyl phthalate (MINP) and monobenzyl phthalate (MBz)) in human urine. Human urine samples were subjected to enzymatic deconjugation of the glucuronides followed by extraction with hexane. The extracted phthalate monoesters were methylated with diazomethane, purified on a Florisil column and then subjected to GC-MS analysis. The recoveries from urine spiked with five phthalate monoesters were 86.3%-119% with coefficients of variation of 0.6%-6.1%. We measured phthalate monoester levels in human urine by analyzing 36 samples from volunteers. MBP and MEP were detected in all samples, and their median concentrations were 60.0 and 10.7 ng/mL, respectively. MBzP and MEHP were found in 75% and 56% of samples, and their median concentrations were 10.9 and 5.75 ng/mL, respectively. MINPs were not detected in most samples (6% detectable). Women had significantly (p < 0.05) higher mean concentrations of MBP and MEP than men. The estimated daily exposure levels for the four parent phthalates excluding diisononyl phthalate ranged from 0.27 to 5.69 mug/kg/day (median).

摘要

我们开发了一种气相色谱-质谱(GC-MS)方法来测定人尿中的五种邻苯二甲酸单酯(邻苯二甲酸单乙酯(MEP)、邻苯二甲酸单丁酯(MBP)、邻苯二甲酸单(2-乙基己基)酯(MEHP)、邻苯二甲酸单异壬酯(MINP)和邻苯二甲酸单苄基酯(MBzP))。人尿样品经酶促去结合反应生成葡萄糖醛酸苷,然后用正己烷提取。提取的邻苯二甲酸单酯用重氮甲烷甲基化,在 Florisil 柱上纯化,然后进行 GC-MS 分析。用五种邻苯二甲酸单酯对尿样进行加标回收,回收率为 86.3%-119%,变异系数为 0.6%-6.1%。我们通过分析 36 名志愿者的尿液样本,测量了人尿中邻苯二甲酸单酯的水平。所有样品均检测到 MBP 和 MEP,其中位数浓度分别为 60.0 和 10.7 ng/mL。75%和 56%的样品中检出 MBzP 和 MEHP,其中位数浓度分别为 10.9 和 5.75 ng/mL。大多数样品(6%可检出)中未检出 MINP。女性的 MBP 和 MEP 平均浓度明显高于男性(p<0.05)。不包括二异壬基邻苯二甲酸的四种母体邻苯二甲酸的估计每日暴露水平范围为 0.27 至 5.69 mug/kg/天(中位数)。

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