Quantitative and Confirmatory Analysis of Pesticide Residues in Cereal Grains and Legumes by Liquid Chromatography–Quadrupole-Time-of-Flight Mass Spectrometry

Abstract

For controlling pesticide residues in food and ensuring food safety, multiresidue methods that can monitor a wide range of pesticides in various types of foods are required for regulatory monitoring. In this study, to demonstrate the applicability of liquid chromatography–quadrupole time-of-flight mass spectrometry (LC–QTOF-MS) for quantitative and confirmatory analysis of pesticide residues in cereal grains and legumes, the LC–QTOF-MS method using full-scan acquisition was validated for 151 pesticides in brown rice, soybeans, and peanuts at a spiked level of 0.01 mg/kg. With the exception of 5 out of 151 target pesticides, sufficiently high signal intensities were obtained at 0.005 μg/mL (corresponding to 0.01 mg/kg). Trueness was in the range 70–95%, with intra- and inter-day precisions below 16% and 24%, respectively, with the exception of 7 pesticides in brown rice, 10 pesticides in soybeans, and 9 pesticides in peanuts. No interfering peaks were observed near the retention times of the target pesticides. Furthermore, information on accurate fragment-ion masses obtained by a data-independent acquisition enabled unambiguous confirmation. The results suggest that the LC-QTOF-MS method is suitable for pesticide residues’ analysis of cereal grains and legumes, and can be utilized for regulatory routine analysis.