Determination of six carbamate pesticides in leafy vegetables by QuEChERSultra-high performance liquid chromatography-tandem mass spectrometry
Objective An ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)based on QuEChERS method was established for the detection of 6 kinds of carbamate pesticide residues in locally grown leafy vegetables in Ankang city,including aldicarb,aldicarb sulfone,aldicarb sulfoxide,carbofuran,3-hydroxy carbofuran and propoxur.Methods The samples were crushed for extraction with acetonitrile,and then cleaned up by dispersive solid-phase extraction.The carbamate pesticides were separated on an Agilent EC-C18 column(5 μm;150 mm ×2.1 mm).The analytes were detected by electrospray ionization(ESI)in a positive ion multiple reaction mode(MRM)and they were qualitatively determined by retention time and mass spectrum characteristic fragment ion abundance ratio,and quantitatively determined with external standard method.Results Six kinds of carbamate pesticides showed good linearity in the range of 5 ng/ml-500 ng/ml,with the correlation coefficients(r)greater than 0.998.The detection limit of the method was within 0.001 7 mg/kg-0.003 3 mg/kg,and the average recovery rate was within range of 85.2％-105.4％,with the spiked levels of 0.01 mg/kg,0.1 mg/kg and 2.00 mg/kg,and the relative standard deviation(RSD)was within 2.39％-6.95％.Carbo-furan was detected in 3 samples and 3-hydroxy carbofuran was detected in 1 sample from 98 leafy vegetable samples,and the detection rate was 4.08％.There was no sample exceeding the limits and the other pesticides were not detected.It showed a low detection rate and good overall situation.Conclusion The method is rapid,simple,sensitive and accurate for the simultaneous detection of 6 kinds of carbamate pesticide residues in leafy vegetables,which provides technical support for the quality and safety work of analyzing primary agricultural products.
QuEChERSUltra-high performance liquid chromatography-tandem mass spectrometryLeafy vegetablesCar-bamates pesticidePesticide residues
NETL
NSTL
万方数据
维普
