Determination of multi-pesticide residues in vegetable products using a "reduced-scale" Quechers method and flow-modulated comprehensive two-dimensional gas chromatography-triple quadrupole mass spectrometry

J Chromatogr A. 2021 May 24:1645:462126. doi: 10.1016/j.chroma.2021.462126. Epub 2021 Apr 1.

Abstract

The aim of the present research was the development of an analytical method for the determination of multi-pesticide residues (88 target analytes) in four vegetable products (tomatoes, cucumbers, sweet red peppers and iceberg lettuce) using a "reduced-scale" QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction method and flow-modulated comprehensive two-dimensional gas chromatography-triple quadrupole mass spectrometry. In particular, the suitability of flow modulation [with relatively high second-dimension gas flow conditions (8 mL min-1)] for trace analyte determination was evaluated. The samples were prepared according to the QuEChERS procedure as reported by the official European Union method, namely EN 15662:2018, based on the use of 3 g of vegetable product. Matrix-matched calibration processes were carried out for all the samples. The figures-of-merit determined were recovery, linearity, precision, limits of detection (LoDs), and limits of quantification (LoQs). Specifically, recoveries were in the 53-160% range, regression coefficients were between 0.9156 and 0.9999, the LoDs were in the 0.1-6.3 μg kg-1 range, the LoQs were in the 3.0-21.0 μg kg-1 range, and coefficients of variation were between 1 and 28% (at the 50 μg kg-1 level).

Keywords: Comprehensive two-dimensional gas chromatography; Food analysis; Pesticides; QuEChERS; Triple quadrupole mass spectrometry.

MeSH terms

  • Gas Chromatography-Mass Spectrometry / methods*
  • Limit of Detection
  • Pesticide Residues / analysis*
  • Reproducibility of Results
  • Vegetables / chemistry*

Substances

  • Pesticide Residues