首页> 中文期刊>分析测试学报 >QuEChERS提取与高效液相色谱-电喷雾电离串联质谱联用法检测茶叶中的19种农药残留

QuEChERS提取与高效液相色谱-电喷雾电离串联质谱联用法检测茶叶中的19种农药残留

     

摘要

建立了高效液相色谱-电喷雾电离串联质谱同时检测茶叶中阿维菌素、啶虫脒、涕灭威、甲萘威、克百威、萎锈灵、除虫脲、烯酰吗啉、唑螨酯、吡虫啉、茚虫威、甲霜灵、灭多威、腈菌唑、咪酰胺、丙环唑、鱼藤酮、西玛津、戊唑醇19种农药残留的方法.试样经QuEChERS方法进行前处理,超高效液相色谱-电喷雾电离串联质谱法测定,外标法定量.除虫脲的质量浓度在5~75 μg/L范围内线性关系良好,定量下限为50 μg/kg,其余18种分析物的质量浓度均在1~15 μg/L范围内线性关系良好,定量下限均为10μg·kg-1,相关系数均大于0.996,平均加标回收率为68%~105%,相对标准偏差为0.81%~ 15%.该方法简便、可靠、稳定,可用于茶叶中多种农药残留的快速检测与确证.%A multiresidue method was developed for the simutaneous determination of 19 pesticides in tea by LC - MS/MS. The ionisation mode used was positive mode with multiple reaction monitoring. The one precursor/two product ion transitions were used for each neonicotinoids. The procedure, based on QuEChERS prior to the determination by UPLC - MS/MS, was validated based on the SAN-CO European Guidelines with satisfactory spiked recovery (68% - 105% ) and measurement uncertainty (≤20% ). The results showed that the calibration curves were linear in the range of 1 -15 μg/L for 18 analytes and 5 -75 μg/L for difulubenzuron. The limits of quantitation (LOQ) were 50 μg · Kg-1 for difulubenzuron and 10 μg · Kg-1 for the other 18 pesticides. The method was simple, rapid and accurate, and could meet the requirement of the maximum residue limits ( MRLs) for pesticides in tea as recommended by the European Union.

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