[Validation study of a method for multiresidue analysis of pesticides in cereals and pulses using supercritical fluid extraction]

Shokuhin Eiseigaku Zasshi. 2012;53(6):278-90. doi: 10.3358/shokueishi.53.278.
[Article in Japanese]

Abstract

Supercritical fluid extraction (SFE) was applied to extraction of pesticides from cereals and pulses. Residues were extracted from homogenized samples mixed with water-absorbent polymer and supercritical carbon dioxide in a stainless steel tube, followed by elution with acetonitrile. Co-extractives were removed by means of mini-column clean-up. Measurement was performed by GC-MS/MS. Calibration was achieved by preparing matrix-matched calibration standards to counteract matrix effects. With the Japanese method validation guideline for pesticide residues as a reference, the method was assessed in 5 agricultural products spiked with 334 pesticides at 0.01 and 0.1 µg/g. Compounds at each level were extracted from 2 samples on 5 separate days. The trueness of the method for 137 pesticides in all samples was 70-120%, and the repeatability and within-run reproducibility were also consistent with the guideline. The trueness of the method for the other 101 pesticides was in the range of 50-70%, though the repeatability and within-run reproducibility were satisfactory. This method is available as a multiresidue analysis method for cereals and pulses.

Publication types

  • Validation Study

MeSH terms

  • Edible Grain / chemistry*
  • Fabaceae / chemistry*
  • Food Analysis / methods*
  • Gas Chromatography-Mass Spectrometry / methods*
  • Mass Spectrometry / methods*
  • Pesticide Residues / analysis*
  • Pesticide Residues / isolation & purification
  • Reproducibility of Results

Substances

  • Pesticide Residues