Determination of Multiresidue Pesticides in Botanical Dietary Supplements Using Gas Chromatography-Triple-Quadrupole Mass Spectrometry (GC-MS/MS)

J Agric Food Chem. 2016 Aug 10;64(31):6125-32. doi: 10.1021/acs.jafc.6b00746. Epub 2016 May 26.

Abstract

A simplified sample preparation method in combination with gas chromatography-triple-quadrupole mass spectrometry (GC-MS/MS) analysis was developed and validated for the simultaneous determination of 227 pesticides in green tea, ginseng, gingko leaves, saw palmetto, spearmint, and black pepper samples. The botanical samples were hydrated with water and extracted with acetonitrile, magnesium sulfate, and sodium chloride. The acetonitrile extract was cleaned up using solid phase extraction with carbon-coated alumina/primary-secondary amine with or without C18. Recovery studies using matrix blanks fortified with pesticides at concentrations of 10, 25, 100, and 500 μg/kg resulted in average recoveries of 70-99% and relative standard deviation of 5-13% for all tested botanicals except for black pepper, for which lower recoveries of fortified pesticides were observed. Matrix-matched standard calibration curves revealed good linearity (r(2) > 0.99) across a wide concentration range (1-1000 μg/L). Nine commercially available tea and 23 ginseng samples were analyzed using this method. Results revealed 36 pesticides were detected in the 9 tea samples at concentrations of 2-3500 μg/kg and 61 pesticides were detected in the 23 ginseng samples at concentrations of 1-12500 μg/kg.

Keywords: Carbon X/PSA; Carbon X/PSA/C18 SPE; botanicals; dual-phase SPE; multipesticide residue; triple-phase SPE GC-MS/MS.

Publication types

  • Evaluation Study

MeSH terms

  • Dietary Supplements / analysis*
  • Drug Contamination
  • Gas Chromatography-Mass Spectrometry / methods*
  • Ginkgo biloba / chemistry
  • Panax / chemistry
  • Pesticide Residues / analysis*
  • Pesticide Residues / isolation & purification
  • Piper nigrum / chemistry
  • Plant Extracts / chemistry
  • Plant Preparations / analysis*
  • Serenoa
  • Solid Phase Extraction

Substances

  • Pesticide Residues
  • Plant Extracts
  • Plant Preparations
  • saw palmetto extract