一种用于同时分析人尿中农药多残留的定量串联质谱和简化 QuEChERS 方法。
A Quantitative Tandem Mass Spectrometry and Scaled-Down QuEChERS Approach for Simultaneous Analysis of Pesticide Multiresidues in Human Urine.
机构信息
Pesticide Chemistry and Toxicology Laboratory, Department of Agricultural Biotechnology and Research Institute of Agriculture and Life Sciences, Seoul National University, Seoul 08826, Korea.
Drug Metabolism and Bioanalysis Laboratory, College of Pharmacy, The Catholic University of Korea, Bucheon-si, Gyeonggi-do 14662, Korea.
出版信息
Molecules. 2019 Apr 4;24(7):1330. doi: 10.3390/molecules24071330.
Multiresidual pesticide determination in a biological sample is essential for an immediate decision and response related to various pesticide intoxications. A rapid and simultaneous analytical method for 260 pesticides in human urine was developed and validated using liquid chromatography-tandem mass spectrometry (LC-MS/MS). High speed positive/negative switching electrospray ionization (ESI) mode was used, and scheduled multiple reaction monitoring (MRM) was optimized. Three versions of scaled-down QuEChERS procedures were evaluated, and the procedure using non-buffer reagents (magnesium sulfate and sodium chloride) and excluding cleanup steps was selected for optimum pesticide extraction. The limit of quantitation (LOQ) in this methodology was 10 ng/mL for each target pesticide, and correlation coefficient (r²) values of calibration curves were ≥0.988 (linearity range; 10-250 ng/mL). In accuracy and precision tests, the relative error ranges were -18.4% to 19.5%, with relative standard deviation (RSD) 2.1%-19.9% at an LOQ level (10 ng/mL), and -14.7% to 14.9% (RSD; 0.6%-14.9%) at higher concentrations (50, 150, and 250 ng/mL). Recovery range was 54.2%-113.9% (RSD; 0.3%-20.0%), and the soft matrix effect (range; -20% to 20%) was observed in 75.4% of target pesticides. The established bioanalytical methods are sufficient for application to biomonitoring in agricultural exposures and applicable in the forensic and clinic.
多残留农药在生物样本中的测定对于与各种农药中毒相关的即时决策和应对至关重要。本研究采用液相色谱-串联质谱法（LC-MS/MS）建立并验证了一种快速、同时测定人尿液中 260 种农药的分析方法。采用高速正负切换电喷雾电离（ESI）模式，并优化了预定的多重反应监测（MRM）。评价了三种简化的 QuEChERS 方法，选择不使用缓冲试剂（硫酸镁和氯化钠）且不进行净化步骤的方法，以获得最佳的农药提取效果。该方法的定量限（LOQ）为每个目标农药 10ng/mL，校准曲线的相关系数（r²）值≥0.988（线性范围：10-250ng/mL）。在准确度和精密度测试中，相对误差范围为-18.4%至 19.5%，相对标准偏差（RSD）在 LOQ 水平（10ng/mL）为 2.1%-19.9%，在较高浓度（50、150 和 250ng/mL）下为-14.7%至 14.9%（RSD；0.6%-14.9%）。回收率范围为 54.2%-113.9%（RSD；0.3%-20.0%），在 75.4%的目标农药中观察到软基质效应（范围：-20%至 20%）。所建立的生物分析方法足以应用于农业暴露的生物监测，并且适用于法医和临床。
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