Two analytical methods for the simultaneous determination of 20 pesticide residues in rice were proposed.The rice samples were initially extracted with acetonitrile(MeCN), then cleaned up by C18 SPE column(method 1) and QuEChERS method(method 2),respectively. The extract was analyzed by GC-MS/MS under selective reaction monitoring(SRM) mode,in which the pesticides were identified by retention time,selected ions and their relative abundances,and quantified by the external standard method.The results indicated that the linear ranges of pesticides were between 0.01μg/mL and 0.2μg/mL,with correlation coefficients all above 0.99.At three spiked concentration levels( 0.01,0.05,0.20mg/kg),the average recoveries of 20 pesticides in rice purified by method 1 ranged from 63.3% to 96.0%,with relative standard deviations(RSDs) of 1.9%-13.9%.The average recoveries of 20 pesticides in rice purified by method 2 ranged from 67.7% to 121.0%,with RSDs of 1.9%-16.4%.The results showed that there was no obvious difference between two pretreatement methods,and this study provided a different pretreatment way for pesticide residue detection.The proposed method was suitable for the simultaneous determination of multiple pesticide residues in rice.
关键词
大米农药残留气相色谱-串联质谱(GC-MS/MS)QuEChERS固相萃取(SPE)
Keywords
ricepesticide residuesgas chromatography-tandem mass spectrometry(GC-MS/MS)QuEChERSsolid phase extraction(SPE)