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A proof‐of‐concept of parallel single‐drop microextraction for the rapid and sensitive biomonitoring of pesticides in urine
Journal of Separation Science ( IF 2.8 ) Pub Date : 2021-02-17 , DOI: 10.1002/jssc.202001157
Gabriela Mafra 1 , Camila Will 1 , Ricardo Huelsmann 1 , Josias Merib 2 , Eduardo Carasek 1
Affiliation  

In this study, a lab‐made parallel single‐drop microextraction methodology using the magnetic ionic liquid trihexyltetradecylphosphonium tetrachloromanganate (II) as extraction solvent was developed to determine the pesticides tebuconazole, pendimethalin, dichlorodiphenyltrichloroethane, and dichlorodiphenyldichloroethylene in human urine samples. The experimental setup consisted of a 96‐well plate system containing a set of magnetic pins that allowed for the manipulation of up to 96 samples simultaneously, providing an enhanced drop stability compared to traditional single‐drop microextraction approaches. The optimal conditions employed 5.38 ± 0.55 mg of extraction solvent, 1.5 mL of diluted urine samples (1:10), extraction time of 130 min, and subsequent dilution in 20 μL of acetonitrile. The method exhibited satisfactory analytical performance, with limits of detection of 7.5 μg/L for all analytes and coefficients of determination higher than 0.9955. Intraday and interday precisions ranged from 3 to 17% (n = 3) and 15 to 18% (n = 9), respectively, with relative recovery of analytes ranging from 70 to 122%. The method proposed was successfully applied in two human urine samples and no sign of the analytes was detected. The results demonstrated that the proposed method allowed for cost‐effective and high‐throughput methodology to be explored as a valuable tool in bioanalytical applications.

中文翻译:

用于尿液中农药快速灵敏生物监测的平行单滴微萃取概念验证

本研究开发了一种实验室制造的平行单滴微萃取方法,使用磁性离子液体三己基十四烷基四氯锰酸鏻 (II) 作为萃取溶剂,用于测定人尿样品中的农药戊唑醇、二甲戊灵、二氯二苯基三氯乙烷和二氯二苯基二氯乙烯。实验装置由一个 96 孔板系统组成,该系统包含一组磁针,可同时处理多达 96 个样品,与传统的单滴微萃取方法相比,提供了增强的滴稳定性。最佳条件采用 5.38 ± 0.55 mg 提取溶剂、1.5 mL 稀释尿样 (1:10)、提取时间 130 分钟,随后用 20 μL 乙腈稀释。该方法表现出令人满意的分析性能,所有分析物的检测限为 7.5 μg/L,测定系数高于 0.9955。日内和日间精密度范围分别为 3% 至 17% (n = 3) 和 15% 至 18% (n = 9),分析物的相对回收率为 70% 至 122%。所提出的方法已成功应用于两个人类尿液样本,但未检测到分析物的迹象。结果表明,所提出的方法允许将具有成本效益和高通量的方法作为生物分析应用中的一种有价值的工具进行探索。所提出的方法已成功应用于两个人类尿液样本,但未检测到分析物的迹象。结果表明,所提出的方法允许将具有成本效益和高通量的方法作为生物分析应用中的一种有价值的工具进行探索。所提出的方法已成功应用于两个人类尿液样本,但未检测到分析物的迹象。结果表明,所提出的方法允许将具有成本效益和高通量的方法作为生物分析应用中的一种有价值的工具进行探索。
更新日期:2021-02-17
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