Laboratório de Toxicologia e Essencialidade de Metais, Faculdade de Ciências Farmacêuticas de Ribeirão Preto, Universidade de São Paulo, 14049-903, Ribeirão Preto, SP, Brazil.
Laboratório de Toxicologia e Essencialidade de Metais, Faculdade de Ciências Farmacêuticas de Ribeirão Preto, Universidade de São Paulo, 14049-903, Ribeirão Preto, SP, Brazil; Instituto de Ciências Ambientais, Químicas e Farmacêuticas, Universidade Federal de São Paulo, Rua Prof. Artur Riedel, 275, Diadema, SP, 09972-270, Brazil.
Chemosphere. 2020 Feb;240:124951. doi: 10.1016/j.chemosphere.2019.124951. Epub 2019 Sep 23.
A high demand exists in human biomonitoring studies for reliable and straightforward methods that generate data faster and simultaneously. Thus, the present study combines microextraction by packed sorbent (MEPS) and liquid chromatography coupled to mass spectrometry (LC-MS/MS) for simultaneous extraction and determination of various classes of endocrine-disrupting chemicals (EDCs), including parabens, benzophenones, bisphenols, and the antimicrobial, triclocarban in human urine samples. Optimized MEPS conditions were: i) MEPS sorbent (C18), ii) pH of sample (3), iii) volume of sample (250 μL), iv) number of draws-eject cycles (5) and (vi) desorption solvent conditions (100 μL of CHOH:HO 80:20 v/v). The calibration curves were linear over the selected ranges for all studied compound, with correlation coefficients higher than 0.99. The variation coefficient for precision was lower than 20% at lower concentrations and lower than 15% at the higher concentrations studied. The accuracy ranged from 90% to 118%. The proposed strategy affords several advantages over currently published approaches, including simplicity of operation and reduction of sample and solvent volumes and time for matrix clean-up. Moreover, the analytical performance of each MEPS cartridge remained stable over the analysis of at least 70 samples (RSD < 10%). Thus, the current procedure may be an interesting high-throughput alternative for large routine human biomonitoring studies. Urinary geometric mean concentrations of EDCs obtained in this study were close than those previously reported for Brazilian children.
在人体生物监测研究中，人们对能够更快、同时生成数据的可靠且直接的方法存在强烈需求。因此，本研究将填充固相微萃取（MEPS）与液相色谱-质谱联用（LC-MS/MS）相结合，用于同时提取和测定各种类别的内分泌干扰化学物质（EDCs），包括在人体尿液样品中的防腐剂、二苯甲酮、双酚和抗菌剂三氯生。优化后的 MEPS 条件为：i）MEPS 吸附剂（C18）、ii）样品 pH 值（3）、iii）样品体积（250 μL）、iv）抽提-洗脱循环次数（5）和 v）洗脱溶剂条件（100 μL 的 CHOH:HO 80:20 v/v）。所有研究化合物的校准曲线在选定范围内均呈线性，相关系数均高于 0.99。在较低浓度下，精密度的变异系数低于 20%，在较高浓度下，精密度的变异系数低于 15%。准确度在 90%至 118%之间。与目前已发表的方法相比，该策略具有多个优势，包括操作简单、减少样品和溶剂体积以及用于基质净化的时间。此外，至少分析 70 个样本后，每个 MEPS 萃取小柱的分析性能仍保持稳定（RSD<10%）。因此，目前的程序可能是用于大型常规人体生物监测研究的一种很有前途的高通量替代方法。本研究中获得的 EDC 几何平均浓度与之前报道的巴西儿童的浓度接近。
