苹果中痕量吡虫啉农药的固相萃取及高效液相色谱-串联质谱分析  

Trace Determination of Imidacloprid Residues in Apple by Solid Phase Extraction Combine with High Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：李俊芳[1] 杜光明[1] 李德强[1] 加列西.马那甫 

机构地区：[1]新疆农业大学化学工程学院,乌鲁木齐830052

出　　处：《农药》2016年第3期194-197,213,共5页Agrochemicals

基　　金：新疆农业大学校前期资助项目(XJAU201302)

摘　　要：[目的]构建一种固相萃取-液相色谱-串联质谱技术测定苹果中痕量吡虫啉残留量的方法。[方法]采用1%的醋酸-乙腈溶液为提取剂,以乙二胺-N-丙基硅烷（PSA）和硅胶（C18E）为分散净化剂的固相萃取方法提取苹果中的吡虫啉,并利用高效液相色谱-串联质谱法（HPLC-MS/MS）法进行检测。[结果]吡虫啉在0.005~1.0 mg/L之间呈良好的线性关系,线性相关系数为0.999 97;检出限（LOD）为0.0119 mg/kg;定量限（LOQ）为0.0397 mg/kg;在0.01、0.05、0.1 mg/kg三个添加水平上,苹果中吡虫啉的平均回收率在95%~100%之间,相对标准偏差（RSD）为2.2%~6.8%。[结论]方法操作简单、灵敏度高,满足现行法规要求,可实现苹果中吡虫啉的痕量测定。[Aims] The aims were to established a method of determination of trace imidacloprid residues in apple by solid phase extraction combine with high performance liquid chromatography tandem mass spectrometry. [Methods] The imidacloprid residues in sample were extracted with 1% of acetic acid-acetonitrile solution, cleaned up by ethylenediamine propyl silane（PSA） and C18 E, and detected by HPLC/MS/MS. [Results] The results showed that the linear correlation coefficient was 0.999 97 when the concentration ranged from 0.005 to 1.0 mg/L. The limit of detection（LOD） was 0.0119 mg/kg,and the limit of quantification（LOQ） was 0.0397 mg/kg. When the fortification levels were 0.01, 0.05 and 0.1 mg/kg, the recoveries were 95-100% with relative standard deviations（RSD） of 2.2-6.8%. [Conclusions] The method is simple and sensitive, which can meet the requirements for current regulations and achieving trace determination of imidacloprid in apple.

关 键 词：吡虫啉 高效液相色谱-串联质谱法 痕量测定 苹果 

分 类 号：TQ453[化学工程—农药化工] O657.63[理学—分析化学]