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

作　　者：严晓贤 仝凯旋 朱浙辉 谢瑜杰 吴兴强[1] 常巧英[1] 石志红 范春林[1] 陈辉[1] YAN Xiao-xian;TONG Kai-xuan;ZHU Zhe-hui;XIE Yu-jie;WU Xing-qiang;CHANG Qiao-ying;SHI Zhi-hong;FAN Chun-lin;CHEN Hui(Chinese Academy of Inspection and Quarantine,Beijing 100176,China;College of Chemistry and Materials Science,Hebei University,Baoding 071002,China;Tibet Product Quality Supervision and Inspection Institute,Lhasa 850000,China)

机构地区：[1]中国检验检疫科学研究院,北京100176 [2]河北大学化学与材料科学学院,河北保定071002 [3]西藏自治区产品质量监督检验所,西藏拉萨850000

出　　处：《分析测试学报》2024年第4期590-599,共10页Journal of Instrumental Analysis

基　　金：中国检科院基本科研业务费项目(2023JK001)。

摘　　要：建立了藏茶中88种农药残留的改进QuEChERS/超高效液相色谱-串联质谱(QuEChERS/UPLC-MS/MS)检测方法。藏茶样品以1%乙酸乙腈提取和2 g NaCl盐析处理,经交联聚乙烯基吡咯烷酮(PVPP)、十八烷基键合硅胶(C18)、石墨化炭黑(GCB)净化后,以0.01%甲酸水溶液(含2 mmol/L甲酸铵)和0.01%甲酸甲醇为流动相,采用ACQUITY UPLC BEH C18(50 mm×2.1 mm,1.7µm)色谱柱在15 min内实现分离。在电喷雾正离子模式下,采用多反应监测(MRM)模式检测,基质匹配标准曲线外标法定量。结果表明,藏茶中88种农药在相应质量浓度范围内线性良好(相关系数r≥0.9990),检出限(LOD)和定量下限(LOQ)分别为0.15~3µg/kg和0.5~10µg/kg。在1、2、10倍LOQ 3个加标水平下,平均回收率分别为73.2%~108%、73.2~109%、72.5%~110%,相对标准偏差(RSD)均不大于12%。将该方法应用于12批实际样品检测,所有样品均检出农药,其中有4批次样品中吡虫啉超限量值。该方法灵敏度高、简便快捷,能够满足藏茶中88种农药的快速检测要求。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,1.7µm)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 0.9990 in the corresponding concentration ranges,and the lim⁃its of detection(LODs)and limits of quantitation(LOQs)were in the ranges of 0.15-3µg/kg and 0.5-10µg/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 relative 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 

分 类 号：O657.63[理学—分析化学] TS207.3[理学—化学]