Simultaneous analytical method for 296 pesticide multiresidues in root and rhizome based herbal medicines with GC-MS/MS

PLoS One. 2023 Jul 6;18(7):e0288198. doi: 10.1371/journal.pone.0288198. eCollection 2023.

Abstract

A method for the simultaneous analysis of pesticide multiresidues in three root/rhizome-based herbal medicines (Cnidium officinale, Rehmannia glutinosa, and Paeonia lactiflora) was developed with GC-MS/MS. To determine the concentrations of pesticide residues, 5 g of dried samples were saturated with distilled water, extracted with 10 mL of 0.1% formic acid in acetonitrile/ethyl acetate (7:3, v/v), and then partitioned using magnesium sulfate and sodium chloride. The organic layer was purified with Oasis PRiME HLB plus light, followed by a cleanup with dispersive solid-phase extraction containing alumina. The sample was then injected into GC-MS/MS (2 μL) using a pulsed injection mode at 15 psi and analyzed using multiple reaction monitoring (MRM) modes. The limit of quantitation for the 296 target pesticides was within 0.002-0.05 mg/kg. Among them, 77.7-88.5% showed recoveries between 70% and 120% with relative standard deviations (RSDs) ≤20% at fortified levels of 0.01, and 0.05 mg/kg. The analytical method was successfully applied to real herbal samples obtained from commercial markets, and 10 pesticides were quantitatively determined from these samples.

MeSH terms

  • Gas Chromatography-Mass Spectrometry / methods
  • Pesticide Residues* / analysis
  • Pesticides* / analysis
  • Plant Extracts / chemistry
  • Rhizome / chemistry
  • Solid Phase Extraction / methods
  • Tandem Mass Spectrometry / methods

Substances

  • Pesticides
  • Pesticide Residues
  • Plant Extracts

Grants and funding

This study was supported by a grant (21172MFDS149) from the Ministry of Food and Drug Safety for the draft submission, and there was no additional external funding received for this study during revision period. The funders had no role in study design, data collection and analysis, decision to publish, or preparation of the manuscript.