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中国精品科技期刊2020
朱颖洁,曹燕卿,毛劼,等. QuEChERS前处理结合超高效液相色谱-串联质谱法同时检测茶叶中14种农药残留[J]. 华体会体育,2022,43(12):283−290. doi: 10.13386/j.issn1002-0306.2021090215.
引用本文: 朱颖洁,曹燕卿,毛劼,等. QuEChERS前处理结合超高效液相色谱-串联质谱法同时检测茶叶中14种农药残留[J]. 华体会体育,2022,43(12):283−290. doi: 10.13386/j.issn1002-0306.2021090215.
ZHU Yingjie, CAO Yanqing, MAO Jie, et al. Determination of 14 Pesticide Residues in Tea by QuEChERS Combined with Ultra-performance Liquid Chromatography-tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2022, 43(12): 283−290. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021090215.
Citation: ZHU Yingjie, CAO Yanqing, MAO Jie, et al. Determination of 14 Pesticide Residues in Tea by QuEChERS Combined with Ultra-performance Liquid Chromatography-tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2022, 43(12): 283−290. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021090215.

QuEChERS前处理结合超高效液相色谱-串联质谱法同时检测茶叶中14种农药残留

Determination of 14 Pesticide Residues in Tea by QuEChERS Combined with Ultra-performance Liquid Chromatography-tandem Mass Spectrometry

  • 摘要: 建立了QuEChERS(Quick,Easy,Cheap,Effective,Rugged,Safe)前处理结合超高效液相色谱-串联质谱法(UPLC-MS/MS)测定茶叶中14种农药残留的方法。茶叶样品经含1%乙酸的乙腈提取,QuEChERS净化柱净化后直接进行UPLC-MS/MS测定。比较了4种QuEChERS净化柱对茶叶提取液的净化效果和农药残留的回收率,选取净化效果和回收率最好的净化柱进一步考察方法的基质效应、线性关系、回收率等。结果表明,方法的检出限为0.001~2.000 μg/L,定量限为0.003~5.000 μg/L;14种农药在相应浓度范围内呈良好的线性关系,决定系数R2为0.9926~0.9989。在100、500、800 μg/kg 3个添加水平下14种农药的回收率为71.2%~117.4%,相对标准偏差为1.1%~14.2%。该方法具有操作简单快速、灵敏度高、回收率好等优点,能够满足茶叶中多农残快速检测要求。

     

    Abstract: A method for the determination of 14 pesticide residues in tea was developed by QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) pretreatment combined with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The tea samples were extracted with acetonitrile (with 1% acetic acid), purified using QuEChERS purification columns and then analyzed by UPLC-MS/MS. The effects of four purification columns on tea extracts and the recoveries of pesticide residues were compared. The column with better purification effect and recovery was selected to further investigate the matrix effect, linear relationship, and recovery of the method. The results showed that the detection limit of the method was 0.001~2.000 μg/L, and the limit of quantification was 0.003~5.000 μg/L. Reliable linear relationship within the corresponding concentration range were observed for 14 pesticides, with coefficient of determination between 0.9926 and 0.9989. The average recoveries were 71.2%~117.4% at the spiking levels of 100, 500, and 800 μg/kg with RSDs at the range of 1.1%~14.2%. This method showed its advantages of simple and fast operation, sensitivity and recovery rate, meeting the requirements for determination of multi pesticide residues in tea.

     

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