SPE-GC-MS/MS法测定茶叶中的76种农药残留

SPE-GC-MS/MS Method for the Determination of76 Pesticide Residues in Tea Sample

建立了一种基于固相萃取结合GC-MS/MS的检测方法,该方法采用乙腈作为提取溶剂、石墨化炭黑-氨基复合柱作为净化手段,于GC-MS/MS上进行高灵敏的多反应监测(MRM)模式检测。结果表明,在2~500μg/L范围内(联苯菊酯、六六六和滴滴涕的质量浓度范围为0.5~125.0μg/L),76种农药均具有良好的线性关系,相关系数为0.994 4~0.999 9;除甲胺磷、乙酰甲胺磷外,低、中、高3个水平的加标回收率分别为82.7%~119.5%、78.6%~114.2%、80.4%~109.3%,相对标准偏差(RSD)均低于15%,该检测方法能够较好地满足茶叶样品中多农残的检测要求。

A sensitive and simple method based on solid phase extraction combined with GC-MS/MS was established for the determination of multiple pesticide residues in tea matrix.In this method,tea samples were extracted with acetonitrile and cleaned by GCB/NH2 columns.The multiple reaction monitoring(MRM)mode was implied for sensitively detection on GC-MS/MS.The results showed that in the range of 2~500μg/L(the concentration range of bifenthrin,BHC and DDT was 0.5~125μg/L),all kinds of pesticides had good linear relationships.The correlation coefficients were ranged from 0.9944 to 0.9999;Except for methamidophos and acephate,the recoveries of this method at the three levels of low,medium and high were in the ranges of 82.7%~119.5%,78.6%~114.2%and 80.4%~109.3%,respectively.And the relative standard deviations(RSD)were all less than 15%.Consequently,this detection method can better meet the detection requirements of multiple pesticide residues in tea samples.