封腾望, 王新新, 周锐东, 刘欢, 孙慧武, 李晋成. 滤过型净化柱净化-超高效液相色谱-三重四极杆/复合线性离子阱质谱法测定草鱼中11种农药残留[J]. 农药学学报, 2022, 24(5): 1268-1277. DOI: 10.16801/j.issn.1008-7303.2022.0097
    引用本文: 封腾望, 王新新, 周锐东, 刘欢, 孙慧武, 李晋成. 滤过型净化柱净化-超高效液相色谱-三重四极杆/复合线性离子阱质谱法测定草鱼中11种农药残留[J]. 农药学学报, 2022, 24(5): 1268-1277. DOI: 10.16801/j.issn.1008-7303.2022.0097
    FENG Tengwang, WANG Xinxin, ZHOU Ruidong, LIU Huan, SUN Huiwu, LI Jincheng. Determination of 11 pesticides residues in grass carp using ultra-performance liquid chromatography/quadrupole-linear ion trap mass spectrometry coupled with pass-through clean-up column[J]. Chinese Journal of Pesticide Science, 2022, 24(5): 1268-1277. DOI: 10.16801/j.issn.1008-7303.2022.0097
    Citation: FENG Tengwang, WANG Xinxin, ZHOU Ruidong, LIU Huan, SUN Huiwu, LI Jincheng. Determination of 11 pesticides residues in grass carp using ultra-performance liquid chromatography/quadrupole-linear ion trap mass spectrometry coupled with pass-through clean-up column[J]. Chinese Journal of Pesticide Science, 2022, 24(5): 1268-1277. DOI: 10.16801/j.issn.1008-7303.2022.0097

    滤过型净化柱净化-超高效液相色谱-三重四极杆/复合线性离子阱质谱法测定草鱼中11种农药残留

    Determination of 11 pesticides residues in grass carp using ultra-performance liquid chromatography/quadrupole-linear ion trap mass spectrometry coupled with pass-through clean-up column

    • 摘要: 采用推杆式滤过型净化柱净化,结合超高效液相色谱-三重四极杆/复合线性离子阱质谱仪(UPLC-QTRAP-MS/MS)建立了草鱼样品中11种农药残留的检测方法。以乙腈为提取剂,样品经超声、冷冻、离心后,上清液采用以50 mg PSA为净化填料的推杆式滤过型净化柱进行1次快速净化;超高效液相色谱快速分离,三重四极杆/复合线性离子阱质谱仪进行测定。基质匹配法制作标准曲线,外标法定量。结果表明:11种农药在1.0~50.0 μg/kg内的线性关系良好,相关系数均大于0.99;定量限为1.0~2.0 µg/kg。不同添加水平下的回收率为83%~119%,日内相对标准偏差为2.6%~20%,日间相对标准偏差为0.7%~15%。该方法经济、简便、高效,灵敏度高,重复性好,可作为草鱼中农药残留的日常检测方法。

       

      Abstract: A method was established for determination of 11 pesticide residues in grass carp sample based on cheap analytical filtration syringe (CAFS) clean-up column coupled with ultra-performance liquid chromatography/quadrupole-linear ion trap mass spectrometry (UPLC-QTRAP-MS/MS). Using acetonitrile as extraction solvent, the sample was ultrasonic, frozen and centrifuged, and the supernatant was quickly purified once by CAFS clean-up column with 50 mg PSA. After separated by UPLC, the analytes were determined by QTRAP-MS/MS. Matrix-matched calibration curves and the external standard method was employed for quantification. The results showed that the linear relationships of the 11 pesticides were good within 1.0-50.0 μg/kg, and the correlation coefficients were greater than 0.99. The limit of quantification were 1.0-2.0 μg/kg. The recoveries of 11 pesticides at different spiking levels were 83%-119%, and the intra-day and inter-day relative standard deviations were 2.6%-20% and 0.7%-15%, respectively. The method is economical, simple, efficient, sensitive and reproducible, and could be used as a routine method for the detection of pesticide residues in grass carp.

       

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