Multiresidue determination of 114 multiclass pesticides in flue-cured tobacco by solid-phase extraction coupled with gas chromatography and tandem mass spectrometry

J Sep Sci. 2016 Dec;39(23):4629-4636. doi: 10.1002/jssc.201600914. Epub 2016 Nov 11.

Abstract

A sensitive and robust multiresidue method for the simultaneous analysis of 114 pesticides in tobacco was developed based on solid-phase extraction coupled with gas chromatography and tandem mass spectrometry. In this strategy, tobacco samples were extracted with acetonitrile and cleaned up with a multilayer solid-phase extraction cartridge Cleanert TPT using acetonitrile/toluene (3:1) as the elution solvent. Two internal standards of different polarity were used to meet simultaneous pesticides quantification demands in the tobacco matrix. Satisfactory linearity in the range of 10-500 ng/mL was obtained for all 114 pesticides with linear regression coefficients higher than 0.994. The limit of detection and limit of quantification values were 0.02-5.27 and 0.06-17.6 ng/g, respectively. For most of the pesticides, acceptable recoveries in the range of 70-120% and repeatabilities (relative standard deviation) of <11% were achieved at spiking levels of 20, 100, and 400 ng/g. Compared with the reported multiresidue analytical method, the proposed method provided a cleaner test solution with smaller amounts of pigments, fatty acids as well as other undesirable interferences. The development and validation of the high sensitivity, high selectivity, easy automation, and high-throughput analytical method meant that it could be successfully used for the determination of pesticides in tobacco samples.

Keywords: Gas chromatography with tandem mass spectrometry; Multiresidue analysis; Pesticides; Solid-phase extraction; Tobacco.

MeSH terms

  • Gas Chromatography-Mass Spectrometry*
  • Nicotiana / chemistry*
  • Pesticides / analysis*
  • Solid Phase Extraction*
  • Tandem Mass Spectrometry*

Substances

  • Pesticides