Abstract

In this study, a new rapid cleanup method was developed for the analysis of 111 pesticide multi-residues in lettuce and Chinese chives by GC–MS/MS and LC–MS/MS. QuEChERS (quick, easy, cheap, effective, rugged and safe)-based sample extraction was used to obtain the extracts, and the cleanup procedure was carried out using a Sin-QuEChERS nano cartridge. Comparison of the cleanup effects, limits of quantification and limits of detection, recoveries, precision and matrix effects (MEs) between the Sin-QuEChERS nano method and the classical dispersive solid phase extraction (d-SPE) method were performed. When spiked at 10 and 100 μg/kg, the number of pesticides with recoveries between 90% to 110% and relative standard deviations < 15% were greater when using the Sin-QuEChERS nano method. The MEs of Sin-QuEChERS nano and d-SPE methods ranged between 0.72 to 3.41 and 0.63 to 3.56, respectively. The results verified that the Sin-QuEChERS nano method was significantly more effective at removing pigments and more convenient than the d-SPE method. The developed method with the Sin-QuEChERS nano cleanup procedure was applied successfully to determine pesticide residues in market samples.

Highlights

  • Pesticides prevent and control pests, diseases and weeds and are used to improve vegetable production levels and quality

  • Cartridge A packed with 90 mg primary secondary amine (PSA) and 15 mg Multi-walled carbon nanotubes (MWCNTs) was used for the lettuce sample, and cartridge B packed with 15 mg MWCNTs, 90 mg PSA, 80 mg graphitized carbon black (GCB) and 80 mg C18 was used for the Chinese chives sample

  • The results demonstrate that the Sin-QuEChERS nano cleanup method performed better than dispersive solid phase extraction (d-SPE)

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Summary

Introduction

Pesticides prevent and control pests, diseases and weeds and are used to improve vegetable production levels and quality. The application of pesticides often leaves pesticide residues in vegetables, which represent a health risk to humans and animals. Measuring trace levels of pesticides in vegetables is becoming a challenging task because of the increasing number and variety of pesticides, and the presence of sample matrix components. In the past few decades, many extraction and cleanup methods for removing pesticide residues in vegetables have been developed, such as matrix solid-phase dispersion [1,2], solid phase extraction [3,4]. The QuEChERS method consists of three main steps: extraction with organic solvent, partition with salts and cleanup by dispersive solid phase extraction (d-SPE) with a small quantity of sorbents. In the d-SPE procedure, primary secondary amine (PSA), graphitized carbon black (GCB) and octadecyl-silane (C18 ) are the main sorbents used to adsorb organic acids, and to some extent adsorb various pigments and sugars [5]

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