Multi-residue analytical method for trace detection of new-generation pesticides in vegetables using gas chromatography-tandem mass spectrometry

A GC-MS/MS method with low solvent consumption and easy operation was developed to simultaneously determine ten new-generation pesticides, namely fenobucarb, acetochlor, pretilachlor, fipronil, trifloxystrobin, fluazifop-p-butyl, isoprothiolane, tebuconazole, cypermethrin and difenoconazole in leafy vegetables. Influences from ultrasonic sample extraction and the clean-up steps to reduce matrix effects were investigated. Under suitable conditions, good linearity (deviation of back calculated concentration from true concentration lower than 20%) was achieved for all studied pesticides; the method detection limits (MDLs) ranged from 1.4 to 3.6 ng g(-1) wet weight. For mustard green and green onion the method yielded good recoveries at two spiking levels (20(1) and 100 ng g(-1)) ranging from 80% to 111% (n = 5). The repeatability, expressed as relative standard deviation (RSD), was lower than 11% (n = 5). The method was successfully used to quantify pesticide residues in 207 vegetable samples (green onions, mustard greens, and lettuce) collected in Thua Thien Hue and Quang Binh Provinces, Central Vietnam. The insecticide cypermethrin was found at critical levels in 98% of the vegetable samples. Green onions had high pesticide residues with a significant number of samples containing pesticides at concentrations exceeding the maximum residue levels (MRLs).