GC-MS/MS方法测定卷柏中66种农药残留

Determination of 66 Kinds of Pesticide Residues in Herba Selaginellae by GC-MS/MS

目的:建立同时分析测定卷柏中66种农药残留的GC-MS/MS方法。方法:样品经乙腈提取,采用分散固相萃取净化管净化,氮吹浓缩,定容后过滤。采用GC-MS/MS联用法测定卷柏中的农药残留量。结果:在实验条件下,66种农药组分能很好地分离检测,在相应的测定范围4.8~250 ng·mL-1内线性关系良好,相关系数均大于0.991,各成分的检出限均在0.0005~0.005 mg·kg-1之间,方法的精密度和重复性RSD均小于5%,加标回收率在69.0%~125.7%之间,RSD均小于10%。结论:该方法灵敏度高,快速简便,可用于对卷柏的农药残留测定。

Objective:To establish a method of 66 pesticide residues in Herba Selaginellae based on GC-MS/MS technique.Methods:Samples were extracted with acetonitrile and purified by the small column of SPA,the analysis was performed by GC-MS/MS.Results:All the 66 pesticides showed good linearities in their reasonable rang(4.8-250 ng·mL-1),R 2>0.991,the LODs of each pesticide were all in the range of 0.0005-0.004 mg·kg-1,the RSD of precision and repeatability of the developed method were less than 5%,and the average recoveries of all the pesticides were in the range of 69.0%-125.7%,the RSD were less than 10%.Conclusion:The method is suitable for the multiresidues analysis of pesticides in Herba Selaginellae owing to its advantages of rapidity,simplicity and better sensitivity.