Dispersive solid-phase extraction cleanup combined with accelerated solvent extraction for the determination of carbamate pesticide residues in Radix Glycyrrhizae samples by UPLC-MS-MS

J Chromatogr Sci. 2011 Oct;49(9):702-8. doi: 10.1093/chrsci/49.9.702.

Abstract

Dispersive solid-phase extraction (DSPE) cleanup combined with accelerated solvent extraction (ASE) is described here as a new approach for the extraction of carbamate pesticides in Radix Glycyrrhizae samples prior to UPLC-MS-MS. In the DSPE-ASE method, 15 carbamate pesticides were extracted from Radix Glycyrrhizae samples with acetonitrile by the ASE method at 60 °C with a 5 min heating time and two static cycles. Cleanup of a 1 mL aliquot of the extract by the DSPE method used 20 mg PSA (primary secondary amine), 50 mg Al(2)O(3)-N, and 20 mg GCB (graphitized carbon black) (as cleanup sorbents) under the determined optimum conditions. The linearity of the method was in the range of 10 to 200 ng/mL with correlation coefficients (r(2)) of more than 0.996. The limits of detection were approximately 0.2 to 5.0 µg/kg. The method was successfully used for the analysis of target pesticides in Radix Glycyrrhizae samples. The recoveries of the carbamate pesticides at the spiking levels of 50, 100, and 200 µg/kg ranged from 79.7% to 99.3% with relative standard deviations lower than 10%. This multi-residue analytical method allows for a rapid, efficient, sensitive and reliable determination of target pesticides in Radix Glycyrrhizae and other medicinal herbs.

Publication types

  • Evaluation Study
  • Research Support, Non-U.S. Gov't

MeSH terms

  • Acetonitriles / chemistry
  • Carbamates / isolation & purification*
  • Chromatography, High Pressure Liquid / economics
  • Chromatography, High Pressure Liquid / methods
  • Glycyrrhiza / chemistry*
  • Limit of Detection
  • Pesticide Residues / isolation & purification*
  • Sensitivity and Specificity
  • Solid Phase Extraction / economics
  • Solid Phase Extraction / methods*
  • Spectrometry, Mass, Electrospray Ionization / economics
  • Spectrometry, Mass, Electrospray Ionization / methods
  • Tandem Mass Spectrometry / economics
  • Tandem Mass Spectrometry / methods

Substances

  • Acetonitriles
  • Carbamates
  • Pesticide Residues
  • acetonitrile