Analysis of multi-component pesticide residues in herbal medicines by GC-MS with electron impact ionization and with positive- and negative-ion chemical ionization

Abstract

Multicomponent pesticide residues in herbal medicines have been analyzed by gas chromatography-mass spectrometry (GC-MS) with electron impact (EI) ionization and positive- and negative-ion chemical ionization (PCI and NCI). Herbal medicines (5 g) were extracted with 65∶35 (%,v/v) acetonitrile-water, and partitioned with hexane-diethyl ether (1∶1) and hexane-dichloromethane (1∶1). The organic phase of the extracted fraction was cleaned on a Florisil column and analyzed by GC-MS with selected-ion monitoring (SIM). Method detection limits for 27 pesticides were tens of picograms for ECD, NPD and EI-SIM MS, and a few picograms for NCI-SIM MS. The calibration curve for the pesticide standard solution was linear within the range 0.003–30 pg for EI-SIM MS, PCI-SIM MS, and NCI-SIM MS. Mean recoveries of pesticides from spiked herbal medicines (0.75, 1.5, 3 pg) were 61–125% (RSD1–32%) for NCI-SIM MS and 74–121% (RSD 4–12%) for EI-SIM MS. Detection sensitivity and specificity of NCI-SIM MS were better than for ECD and NPD. Parallel use of EI-SIM MS, PCI-SIM MS and NCI-SIM MS was an excellent complementary method for identification and confirmation of multi-component pesticide residues in variety of herbal medicines.