固相萃取高效液相色谱法测定蔬菜、水果中的氨基甲酸酯杀虫剂及其代谢物残留

Determination of the Multiresidue of Carbamate Insecticides and Their Metabolites in Vegetables and Fruits by Solid-Phase Extraction and High Performance Liquid Chromatography

采用乙腈提取、固相萃取浓缩、高效液相色谱分离、柱后衍生 荧光检测法测定了蔬菜、水果中8种氨基甲酸酯类杀虫剂及其代谢物残留量。采用加标法(添加水平为0 10,0 50mg/kg)测定了氨基甲酸酯杀虫剂及其代谢物的回收率,其平均回收率为70%～120%,相对标准偏差(RSD)小于20%(n=3),最低检出限范围为0 0042～0 0106mg/kg。该方法的测定结果满足多残留农残的检测要求。

A method for the rapid determination of multiresidue of carbamate insecticides and their metabolites by high performance liquid chromatography (HPLC) has been developed. The samples were extracted with acetonitrile and cleaned up with methanoldichlormethane (1∶99, v/v) on an aminopropyl solidphase extraction column. With gradient elution in HPLC, the analytes were quantitated simultaneously by postcolumn derivatization on a fluorescene detector (λex=330 nm, λem=465 nm). The average spiked recoveries ranged from 70% to 120% in 6 vegetables and fruits, and the relative standard deviations were less than 20%. The range of the limit of detection (LOD) was 0004?2-0010?6 mg/kg. 