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一种快速多组分方法,用于通过涡旋辅助分散液液微萃取(VADLLME)和 LC-MS/MS 测定人尿中的 21 种内分泌干扰物。

A fast-multiclass method for the determination of 21 endocrine disruptors in human urine by using vortex-assisted dispersive liquid-liquid microextraction (VADLLME) and LC-MS/MS.

机构信息

Departamento de Análises Clínicas, Toxicológicas e Bromatológicas, Faculdade de Ciências Farmacêuticas de Ribeirão Preto, Universidade de São Paulo, 14040-903, Ribeirão Preto, SP, Brazil.

Faculdade de Ciências Farmacêuticas, Universidade de Ribeirão Preto, 14096-900, Ribeirão Preto, SP, Brazil.

出版信息

Environ Res. 2020 Oct;189:109883. doi: 10.1016/j.envres.2020.109883. Epub 2020 Jul 11.

Abstract

Simplicity, speed, and reduced cost are essential demands for routine analysis in human biomonitoring studies. Moreover, the availability of higher volumes of human specimens is becoming more restrictive due to ethical controls and to the costs associated with sample transportation and storage. Thus, analytical methods requiring much lower sample volumes associated with simultaneous detection capability (multiclass analysis) are with a very high claim. In this sense, the present approach aimed at the development of a method for preconcentration and simultaneous determination of four classes of endocrine disruptors (seven bisphenols, seven parabens, five benzophenones, and two antimicrobials) in the urine. The approach is based on vortex-assisted dispersive liquid-liquid microextraction (VADLLME) and high-performance liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). After optimization of the significant parameters of VADLLME extraction, the proposed procedure showed to be simple, fast, sensitive, requiring only 1.0 mL of urine, 400 μL of organic solvents with a total stirring time of 20 s. Moreover, a variation of inter-day and between-day runs were lower than 10.0% and 11.0%, respectively. Finally, the proposed method was successfully applied to the analysis of 50 urine samples of Brazilian pregnant women to establish reference ranges.

摘要

在人体生物监测研究中,简单、快速和降低成本是常规分析的基本要求。此外,由于伦理控制以及与样本运输和储存相关的成本,可获得的人体标本量越来越受到限制。因此,需要更少样本量且具有同时检测能力(多类分析)的分析方法的需求非常高。从这个意义上说,本研究旨在开发一种方法,用于浓缩和同时测定尿液中的四类内分泌干扰物(七种双酚、七种对羟基苯甲酸酯、五种二苯甲酮和两种抗菌剂)。该方法基于涡旋辅助分散液液微萃取(VADLLME)和高效液相色谱串联质谱联用(LC-MS/MS)。在优化 VADLLME 萃取的重要参数后,所提出的方法简单、快速、灵敏,仅需 1.0 mL 尿液和 400 μL 有机溶剂,总搅拌时间为 20 s。此外,日内和日间运行的变化分别低于 10.0%和 11.0%。最后,该方法成功应用于分析 50 份巴西孕妇的尿液样本,以建立参考范围。

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