摘要
目的建立QuEChERS-超高效液相色谱-串联质谱法测定葡萄中多菌灵等100种农药及其代谢物的分析方法。方法样品采用1%乙酸乙腈涡旋振荡提取,离心后取上清液用N-丙基乙二胺(N-propylethylenediamine,PSA)粉末分散固相萃取净化,样品经BEH-C18超高效液相色谱柱分离后,在电喷雾正离子(electrosprayionization,ESI+)模式下,通过多反应监测(multiplereactionmonitoring,MRM)模式测定,以基质匹配校准曲线外标法进行定量分析。结果100种农药及其代谢物在1~100μg/L范围内线性关系良好,相关系数(r2)均大于0.9984;100种农药及代谢物的平均回收率在77.6%~118.4%之间,相对标准偏差为0.3%~28.9%,符合农药多残留分析的要求。结论本方法简单、灵敏,适用于葡萄中100种农药及其代谢物的准确测定。
Objective To establish an analytical method for the determination of carbendazim and other 100 kinds of pesticides and their metabolites including carbendazim in grape by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry.Methods The samples were extracted with 1%acetonitrile acetate by vortex oscillation,and the supernatant after centrifugation was purified by N-propylethylenediamine(PSA)powder dispersion solid-phase extraction.After the samples were separated by BEH-C18 ultra-performance liquid chromatographic column,the samples were collected under the electrospray ionization(ESI+)mode,quantitation was performed using a matrix-matched calibration curve external standard,as determined by multiple reaction monitoring(MRM)mode.Results The linear relationships were good in the range of 1-100μg/L,and the correlation coefficients(r2)were greater than 0.9984.The average recoveries of the 100 kinds of pesticides and theirs metabolites were 77.6%-118.4%,and the relative standard deviations were 0.3%-28.9%,which met the requirements of multi-residue analysis of pesticides.Conclusion This method is simple,sensitive and suitable for the accurate determination of 100 kinds of pesticides and their metabolites in grapes.
作者
苏漪玲
吴延灿
戚传勇
操海群
檀根甲
董玉平
师焕芝
SU Yi-Ling;WU Yan-Can;QI Chuan-Yong;CAO Hai-Qun;TAN Gen-Jia;DONG Yu-Ping;SHI Huan-Zhi(Hefei Inspection Center for Agricultural Products Quality,Hefei 230091,China;College of Plant Protection,Anhui Agricultural University,Hefei 230036,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2021年第16期6528-6536,共9页
Journal of Food Safety and Quality
基金
合肥市农产品质量安全体系首席专家工作室项目~。