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超高效液相色谱-串联质谱法测定人乳中 9 种双酚基二缩水甘油醚

Determination of Nine Bisphenol-Diglycidyl Ethers in Human Breast Milk by Ultrahigh-Performance Liquid Chromatography Tandem Mass Spectrometry.

机构信息

College of Food Engineering and Biotechnology , Tianjin University of Science and Technology , Tianjin 300457 , China.

Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning , Beijing Center for Disease Prevention and Control , Beijing 100013 , China.

出版信息

J Agric Food Chem. 2018 Sep 19;66(37):9810-9818. doi: 10.1021/acs.jafc.8b03088. Epub 2018 Sep 7.

DOI:10.1021/acs.jafc.8b03088
PMID:30148360
Abstract

Because of their widespread use, and the mutagenicity and teratogenicity observed in in vitro studies, bisphenol-diglycidyl ethers (BDGEs) were suspected of posing health risks to humans, especially to infants. Quantifying exposure of BDGEs from breast milk is essential in assessing the potential health risks of these ubiquitous compounds to infants. However, there is no reported analytical method for the determination of BDGEs in breast milk. In this context, we developed a rapid and sensitive method based on ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) to measure nine BDGEs in breast milk. The analytes were extracted with acetonitrile and fat was removed by freezing under -20 °C. The extracts were further purified by PRiME HLB solid-phase extraction (SPE) cartridge. The limits of detection (LODs) and quantification (LOQs) for the analytes were 0.033-0.500 and 0.100-1.500 μg L, respectively. The recoveries of BDGEs were ranged from 71.33% to 114.33%. Good method reproducibility regarding intra- and interday precision was observed, yielding relative standard deviations (RSDs) less than 11.81% and 10.83%, respectively. The proposed method was successfully applied to 20 breast milk samples. BADGE·2HO, BADGE·HCl·HO, BADGE·HO, BADGE·HCl, BFDGE·2HO, and BFDGE·2HCl were detected. BFDGE·2HCl was the dominant BDGE with detection rate of 65.0% and the concentration ranging from 0.4 to 1.0 μg L. This is the first report describing the occurrence of BDGEs in breast milk.

摘要

由于双酚 - 二缩水甘油醚(BDGE)广泛使用,并且在体外研究中观察到其致突变性和致畸性,因此怀疑其对人类健康构成风险,尤其是对婴儿。定量测定母乳中 BDGE 的含量对于评估这些普遍存在的化合物对婴儿的潜在健康风险至关重要。然而,目前尚无报道用于测定母乳中 BDGE 的分析方法。在这种情况下,我们开发了一种基于超高效液相色谱 - 串联质谱(UPLC-MS/MS)的快速灵敏方法,用于测定母乳中的 9 种 BDGE。用乙腈提取分析物,并用 -20°C 冷冻去除脂肪。通过 PRiME HLB 固相萃取(SPE)小柱进一步纯化提取物。分析物的检测限(LOD)和定量限(LOQ)分别为 0.033-0.500 和 0.100-1.500 μg/L。BDGE 的回收率在 71.33%-114.33%之间。日内和日间精密度的方法重复性良好,相对标准偏差(RSD)分别小于 11.81%和 10.83%。该方法成功应用于 20 个母乳样本。检测到 BADGE·2HO、BADGE·HCl·HO、BADGE·HO、BADGE·HCl、BFDGE·2HO 和 BFDGE·2HCl。BFDGE·2HCl 是主要的 BDGE,检出率为 65.0%,浓度范围为 0.4-1.0 μg/L。这是首次报道母乳中存在 BDGE 的情况。

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