分析测试学报2024，Vol.43Issue(4)：590-599,10.DOI:10.12452/j.fxcsxb.23121964
改进QuEChERS方法结合超高效液相色谱-串联质谱法快速测定藏茶中88种农药残留
Rapid Determination of 88 Pesticide Residues in Tibetan Tea by Ul-tra Performance Liquid Chromatography-Tandem Mass Spectrome-try Coupled with Improved QuEChERS Method
摘要
Abstract
An improved QuEChERS/ultra performance liquid chromatography-tandem mass spec-trometry(QuEChERS/UPLC-MS/MS)analytical method was developed for the determination of 88 pesticide residues in Tibetan tea.Tibetan tea samples were extracted with 1%acetic acid acetonitrile and salted with 2 g NaCl,cleaned up by polyvinylpyrrolidone(PVPP),octadecyl bonded silica gel(C18)and graphitized carbon black(GCB),and then separated with 0.01%formic acid aqueous solu-tion(containing 2 mmol/L ammonium formate)and 0.01%formic acid methanol as the mobile phas-es.The analytes were separated on an ACQUITY UPLC BEH C18(50 mm×2.1 mm,1.7 μm)col-umn to achieve the separation within 15 min,detected in electrospray positive ionization mode with multiple reaction monitoring(MRM)mode and quantified by matrix matching curve external standard method.The results showed that 88 pesticides in Tibetan tea showed good linear correlations with cor-relation coefficients(r)not less than 0.999 0 in the corresponding concentration ranges,and the lim-its of detection(LODs)and limits of quantitation(LOQs)were in the ranges of 0.15-3 μg/kg and 0.5-10 μg/kg,respectively.Average recoveries of the 88 pesticides in Tibetan tea at three spiked levels(1,2,and 10-fold LOQ)were 73.2%-108%,73.2%-109%,72.5%-110%,and the rela-tive standard deviations(RSDs)were not more than 12%.The method was applied to 12 batches of ac-tual samples and pesticides were detected in all samples,among which 4 batches of imidacloprid ex-ceeded the limit value.The method is sensitive,simple and rapid,and could meet the rapid detec-tion requirements of 88 pesticides in Tibetan tea.关键词
改进QuEChERS/藏茶/超高效液相色谱-质谱法/农药残留Key words
improved QuEChERS/Tibetan tea/ultra performance liquid chromatography-mass spectrometry/pesticide residues分类
化学化工引用本文复制引用
严晓贤,仝凯旋,朱浙辉,谢瑜杰,吴兴强,常巧英,石志红,范春林,陈辉..改进QuEChERS方法结合超高效液相色谱-串联质谱法快速测定藏茶中88种农药残留[J].分析测试学报,2024,43(4):590-599,10.基金项目
中国检科院基本科研业务费项目(2023JK001) （2023JK001）
