Validation of a Multiresidue Analysis Method for 379 Pesticides in Human Serum Using Liquid Chromatography-Tandem Mass Spectrometry

J Agric Food Chem. 2018 Apr 4;66(13):3550-3560. doi: 10.1021/acs.jafc.8b00094. Epub 2018 Mar 21.

Abstract

A screening method for simultaneous analysis of 379 pesticides in human serum was developed using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Electrospray ionization with positive/negative switching mode of LC-MS/MS was adopted, and scheduled multiple reaction monitoring for each target compound was established. The limit of quantitation was 10 ng/mL for 94.5% of the total pesticides, and the correlation coefficients of calibration were ≥0.990 for 93.9% of the pesticides. For the sample preparation, scaled-down QuEChERS were used. Serum (100 μL) was extracted with acetonitrile (400 μL), partitioned with magnesium sulfate (40 mg) and sodium chloride (10 mg), and the upper layer was used for analysis without further cleanup steps. For the accuracy and precision tests, most of the pesticides showed excellent results in intra- and interday conditions. In the recovery tests at 10, 50, and 250 ng/mL, 85.8-91.8% of all target compounds satisfied the recovery range of 70-120% (relative standard deviation ≤20%).

Keywords: LC−MS/MS; QuEChERS; intoxication; multiresidue; pesticide; serum.

Publication types

  • Validation Study

MeSH terms

  • Chromatography, High Pressure Liquid / methods*
  • Humans
  • Pesticides / blood*
  • Pesticides / chemistry
  • Pesticides / isolation & purification
  • Serum / chemistry*
  • Solid Phase Extraction
  • Tandem Mass Spectrometry / methods*

Substances

  • Pesticides