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一种新的液相色谱-串联质谱法测定人胎盘组织样品中对羟基苯甲酸酯类的方法。

A new liquid chromatography-tandem mass spectrometry method for determination of parabens in human placental tissue samples.

机构信息

Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, Campus of Fuentenueva, University of Granada, E-18071 Granada, Spain.

出版信息

Talanta. 2011 May 15;84(3):702-9. doi: 10.1016/j.talanta.2011.01.075. Epub 2011 Feb 4.

Abstract

Endocrine disruptors are a group of organic compounds widely used, which are ubiquitous in the environment and in biological samples. The main effect of these compounds is associated with their ability to mimic or block the action of natural hormones in living organisms, including humans. Parabens (esters of p-hydroxybenzoic acid) belong to this group of compounds. In this work, we propose a new liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to asses the presence of parabens most commonly used in industrial applications (methyl-, ethyl-, propyl- and butyl-paraben) in samples of human placental tissue. The method involves the extraction of the analytes from the samples using ethyl acetate, followed by a clean-up step using centrifugation prior to their quantification by LC-MS/MS using an atmospheric pressure chemical ionization (APCI) interface in the negative mode. Deuterated bisphenol A (BPA-d(16)) was used as surrogate. Found detection limits (LOD) ranged from 0.03 to 0.06 ng g(-1) and quantification limits (LOQ) from 0.1 to 0.2 ng g(-1), while inter- and intra-day variability was under 13.8%. The method was validated using standard addition calibration and a spike recovery assay. Recovery rates for spiked samples ranged from 82% to 108%. This method was satisfactorily applied for the determination of parabens in 50 placental tissue samples collected from women who live in the province of Granada (Spain).

摘要

内分泌干扰物是一组广泛使用的有机化合物,它们在环境和生物样本中无处不在。这些化合物的主要作用与其模拟或阻断生物体内天然激素作用的能力有关,包括人类。对羟基苯甲酸酯(对羟基苯甲酸的酯类)属于这一类化合物。在这项工作中,我们提出了一种新的液相色谱-串联质谱(LC-MS/MS)方法,用于评估在人类胎盘组织样品中最常用于工业应用的几种对羟基苯甲酸酯(甲基对羟基苯甲酸酯、乙基对羟基苯甲酸酯、丙基对羟基苯甲酸酯和丁基对羟基苯甲酸酯)的存在情况。该方法涉及使用乙酸乙酯从样品中提取分析物,然后在离心前进行净化步骤,然后通过大气压化学电离(APCI)接口在负离子模式下使用 LC-MS/MS 进行定量。使用氘代双酚 A(BPA-d(16))作为内标。检测限(LOD)范围为 0.03 至 0.06ng/g,定量限(LOQ)范围为 0.1 至 0.2ng/g,而日内和日间变异性低于 13.8%。该方法通过标准添加校准和加标回收率试验进行验证。加标样品的回收率范围为 82%至 108%。该方法满意地应用于测定来自西班牙格拉纳达省(西班牙)的 50 名妇女胎盘组织样本中的对羟基苯甲酸酯。

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