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An effective and high-throughput analytical methodology for pesticide screening in human urine by disposable pipette extraction and gas chromatography – mass spectrometry
Journal of Chromatography B ( IF 2.8 ) Pub Date : 2018-06-23 , DOI: 10.1016/j.jchromb.2018.06.047
Anderson Luiz Oenning , Josias Merib , Eduardo Carasek

In this paper, the use of disposable pipette extraction (DPX) for the determination of pesticides in human urine in possible cases of poisoning is proposed for the first time. The pesticides studied were oxamyl, propoxur, carbofuran, 3‑hydroxycarbofuran, carbaryl, methiocarb, terbufos, parathion methyl, malathion, chlorpyrifos and endosulfan. The pipette tip used for the extraction of these compounds was commercially acquired. It has a capacity of 5 mL and contains 20 mg of sorbent material (styrene-divinylbenzene). The optimization of the main parameters that can influence the extraction efficiency of this sample preparation technique was performed with univariate and multivariate approaches. The analytes were separated and identified by gas chromatography coupled to mass spectrometry (GC–MS). The optimal extraction conditions were 5 extraction cycles of 30 s and 5 desorption cycles of 15 s with 250 μL of ethyl acetate. Elution of the extract was performed in a vial containing 100 mg of anhydrous sodium sulfate. The method developed was validated, providing correlation coefficients higher than 0.9955 for all analytes, limits of detection (LOD) of 0.76 to 1.52 μg L−1, limits of quantification (LOQ) of 2.5 to 5.0 μg L−1, relative recoveries of 63 to 118%, intra-day precision of 0.7 to 15.3% and inter-day precision of 4.9 to 13.1%. An effective and rapid method for the analysis of human urine for the identification of possible cases of poisoning by pesticides was successful developed.



中文翻译:

一种高效,高通量的一次性移液管萃取和气相色谱-质谱法筛查人尿中农药的分析方法

在本文中,首次提出了使用一次性移液器萃取(DPX)来测定可能中毒的人尿中的农药的方法。所研究的农药为草酰胺,丙草胺,呋喃丹,3-羟基呋喃呋喃,西维因,甲硫威,萜品磷,甲基对硫磷,马拉硫磷,毒死rif和硫丹。用于提取这些化合物的移液器吸头已商业购得。它的容量为5 mL,包含20 mg的吸附剂材料(苯乙烯-二乙烯基苯)。使用单变量和多变量方法对可能影响该样品制备技术的提取效率的主要参数进行了优化。通过气相色谱-质谱联用(GC-MS)分离和鉴定分析物。最佳提取条件是使用250μL乙酸乙酯的5个30 s的提取循环和15 s的5个解吸循环。在含有100mg无水硫酸钠的小瓶中进行提取物的洗脱。所开发的方法经过验证,可为所有分析物提供高于0.9955的相关系数,检测限(LOD)为0.76至1.52μgL-1,定量限(LOQ)为2.5至5.0μgL -1,相对回收率为63至118%,日内精度为0.7至15.3%和日间精度为4.9至13.1%。成功开发了一种有效,快速的人尿分析方法,以鉴定可能的农药中毒病例。

更新日期:2018-06-23
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