An effective, rapid, and simultaneous multi-residue screening method of 380 pesticides in human urine was developed and established using liquid chromatography-tandem mass spectrometry (LC-MS/MS, SHIMADZU LCMS-8050) for forensic and toxicological investigation. The scheduled selected reaction monitoring (SRM) on LC-MS/MS was optimized with positive/negative ionization mode. For the sample preparation, the pesticides in 100 μL of human urine were extracted with acetonitrile (400 μL), treated with magnesium sulfate (40 mg) and sodium chloride (10 mg) in 2 mL tube, and the extracts were centrifuged. And then the extracts (200 μL) were diluted with acetonitrile (50 μL) for matrix matching and analyzed by LC-MS/MS without further clean-up steps. In this methods, the limit of quantitations (LOQs) for 331 (87.1%) compounds were 10 ng/mL, for 27 (7.1%) compounds were 25 ng/mL, and for 22 (5.8%) were ≥50 ng/kg. The correlation coefficients (R<sup>2</sup>) of calibration curves using procedure standard solutions were ≥0.99 for most of target compounds. To evaluate the analytical method developed in this study, the accuracy and the recovery test were carried out. In the accuracy tests, 66.8% of total compounds at 10 ng/mL was between 80-120% with the precision below 20%, and 90.0-96.6% of total compounds at 50, 150, and 250 ng/mL was between 85-115% with the precision below 15%. In the recovery tests at 10, 50 and 250 ng/mL, 75.3-97.1% of all target compounds satisfied the screening method criteria of 50-150% (RSD ≤30%). This established methods can be sufficiently applied for the monitoring of 380 pesticides in urine samples at hospitals and forensic science facilities in need.

Multi-residue screening method for the determination of 380 pesticides in human urine by liquid chromatography-tandem mass spectrometry

253rd National Meeting (2017)

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