Development of an efficient method for multi residue analysis of 160 pesticides in herbal plant by ethyl acetate hexane mixture with direct injection to GC-MS/MS

Abstract

A simple and efficient multi residue method was developed, for the analysis of 160 pesticides by GC-MS/MS in herbal plants. The developed method employs pesticide residue extraction by EtAC/ n. hexane (6:4) with a cleanup step using florisil/ PSA mixture. The optimized conditions have resulted in lower co-extracted matrix components than those extracted using EtAC or MeCN (QuEChERS method), according to FTIR and full scan GC/MS analyses. In addition, the developed method (EtAC/ Hexane) eliminates the evaporation step that is usually performed when using MeCN as an extraction solvent prior to the GC-MS/MS injection. The developed method was fully validated on chamomile, based on SANTE/11945/2015 guidelines. Where, intraday recoveries were estimated at three concentration levels of 10, 50 and 250μgkg−1. However, interday recoveries have also been carried out, at 250μgkg−1. In addition, intraday recoveries were estimated for two other herbal plants (thyme and marjoram), at 250μgkg−1. Three point calibration mixtures were prepared in ethyl acetate solvent and in the blank extracts of chamomile, thyme, and marjoram, in order to check the linearity and matrix effect. The average recoveries for most of the studied pesticides ranged from 70% to 100% at 50 and 250μgkg−1 with relative standard deviations below 20%. The validated method was successfully applied for determination of pesticide residues in 20 herb samples, collected from the Egyptian market.