Simultaneous Determination of Four Pesticides Residues in Vegetables by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. 2016,35(4):476-481.
Simultaneous Determination of Four Pesticides Residues in Vegetables by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. 2016,35(4):476-481.DOI:
A method was developed for the determination of four pesticides residues in a variety of vegetables using solid phase extraction(SPE) and ultra performance liquid chromatography-triple quadrupole-mass spectrometry(UPLC-MS/MS).The purification methods(solid phase extraction column,QuEChERS method,elution solvent,elution volume),chromatographic conditions(mobile phase type,flow rate and column temperature) and mass spectrometric parameters(fragment,delta EMV) were optimized.The pesticides samples were extracted with acetonitrile,and then cleaned up on a Carbon/NH2(or NH2) SPE column.The eluting solution was evaporated and made up to a definite volumn with methanol,finally analyzed by reversed phase ultra performance liquid chromatography under multiple reaction monitoring(MRM) of positive ion mode with the external standard method.The calibration curves of four pesticides showed good linearities in the range of 5-500 μg/L with correlation coefficients not less than 0.999 2.The limits of detection(LOD) were in the range of 0.033-0.167 μg/kg and the limits of quantitation(LOQ) were in the range of 0.10-0.50 μg/kg for 4 pesticides spiked in vegetable.The recoveries of 4 pesticides in vegetable sample spiked with three concentration levels of 10,50,250 μg/kg ranged from 70.9% to 123.4% with RSDs less than 15%.The established method was accurate,sensitive and simple,and was suitable for the simultaneous analysis of various pesticides residues.
关键词
超高效液相色谱-质谱联用固相萃取农药残留蔬菜
Keywords
ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)solid phase extraction(SPE)pesticide residuevegetable