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采用 QuEChERS 提取法的 GC-MS/MS 检测母乳中的 20 种邻苯二甲酸酯

Detection of 20 phthalate esters in breast milk by GC-MS/MS using QuEChERS extraction method.

机构信息

Laboratory of Chemistry and Physics, Hangzhou Center for Disease Control and Prevention , Hangzhou , P. R. China.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2019 Oct;36(10):1551-1558. doi: 10.1080/19440049.2019.1646435. Epub 2019 Jul 30.

Abstract

A detection method for 20 different phthalate esters (PAEs) in breast milk analyzed by quick, easy, cheap, effective, rugged, and safe (QuEChERS) clean-up with five internal standards and quantitative GC-MS/MS was established. This method can effectively remove interfering substances such as lipids and fatty acids from breast milk using acetonitrile as the extraction solvent and PSA/C18 as clean-up materials. The 20 PAEs had a linear range of 5.0-500.0 µg/L and recoveries of 83.3-123.3% with RSDs of 0.2-7.6% (n = 6). The method detection limits (LODs) were 0.004-1.3 µg/kg. Dimethyl phthalate (DMP), Diethyl phthalate (DEP), Diisobutyl phthalate (DIBP), Di-n-butyl phthalate (DBP) and bis(2-ethylhexyl) phthalate (DEHP) were detected in the 35 breast milk samples, with median levels of 1.2, 6.8, 7.3, 32.9 and 13.6 μg/kg, respectively, and the concentrations of 20 PAEs ranged between 0.5 and 137.3 μg/kg. This is a fast, simple, sensitive and accurate method for the detection of 20 PAEs in breast milk or dairy products.

摘要

建立了一种采用快速、简单、廉价、有效、耐用和安全(QuEChERS)净化,并用 5 种内标物和定量 GC-MS/MS 分析母乳中 20 种邻苯二甲酸酯(PAEs)的检测方法。该方法采用乙腈作为提取溶剂,PSA/C18 作为净化材料,能有效去除母乳中的脂类和脂肪酸等干扰物质。20 种 PAEs 的线性范围为 5.0-500.0 µg/L,回收率为 83.3-123.3%,相对标准偏差(RSD)为 0.2-7.6%(n=6)。方法检出限(LODs)为 0.004-1.3 µg/kg。在 35 份母乳样品中检测到二甲酸酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二异丁酯(DIBP)、邻苯二甲酸二正丁酯(DBP)和邻苯二甲酸二(2-乙基己基)酯(DEHP),其浓度中位数分别为 1.2、6.8、7.3、32.9 和 13.6 µg/kg,20 种 PAEs 的浓度范围为 0.5-137.3 µg/kg。该方法快速、简单、灵敏、准确,适用于检测母乳或乳制品中的 20 种 PAEs。

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