QuEChERS-超高效液相色谱-串联质谱法测定葡萄中100种农药及其代谢物

Determination of 100 kinds of pesticides and their metabolites in grapes by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  超高效液相色谱-串联质谱法  葡萄  农药残留  代谢物

英文关键词:QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry  grapes  pesticide residue  metabolites

中文摘要:

      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(electrospray ionization, ESI+)模式下, 通过多反应监测(multiple reaction monitoring, 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1~100 μg/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。

英文摘要:

      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 1-100 μg/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.