杨松, 邹楠, 尤峥, 于杰, 王苓, 宿莉, 慕卫. QuEChERS-超高效液相色谱-串联质谱法检测花生中4种农药残留[J]. 农药学学报, 2021, 23(2): 414-420. DOI: 10.16801/j.issn.1008-7303.2021.0023
    引用本文: 杨松, 邹楠, 尤峥, 于杰, 王苓, 宿莉, 慕卫. QuEChERS-超高效液相色谱-串联质谱法检测花生中4种农药残留[J]. 农药学学报, 2021, 23(2): 414-420. DOI: 10.16801/j.issn.1008-7303.2021.0023
    YANG Song, ZOU Nan, YOU Zheng, YU Jie, WANG Ling, SU Li, MU Wei. Detection of 4 pesticides residues in peanut using QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2021, 23(2): 414-420. DOI: 10.16801/j.issn.1008-7303.2021.0023
    Citation: YANG Song, ZOU Nan, YOU Zheng, YU Jie, WANG Ling, SU Li, MU Wei. Detection of 4 pesticides residues in peanut using QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2021, 23(2): 414-420. DOI: 10.16801/j.issn.1008-7303.2021.0023

    QuEChERS-超高效液相色谱-串联质谱法检测花生中4种农药残留

    Detection of 4 pesticides residues in peanut using QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry

    • 摘要: 建立了超高效液相色谱-串联质谱 (UPLC-MS/MS) 同时检测花生中精喹禾灵、毒死蜱、乙草胺和吡虫啉残留的分析方法。样品以纳米氧化锆 (Nano-ZrO2)、十八烷基键合硅胶 (C18) 和多壁碳纳米管 (MWCNT) 组合进行净化,采用UPLC-MS/MS检测,外标法定量。结果表明:在0.001~0.5 mg/L范围内,4种农药的质量浓度与其对应的峰面积间线性关系良好,r≥0.9986;在0.01、0.1和1 mg/kg 3个添加水平下,4种农药在花生中的平均回收率在82%~109%之间,相对标准偏差 (RSDs,n = 5) 在2.8%~9.0%之间,其定量限 (LOQ) 均为0.01 mg/kg。运用该方法对采自泰安市大型超市和农贸市场的10批次花生样品进行检测,结果表明,所有样品中4种农药的残留量均未超过中国规定的最大残留限量标准。该方法具有净化效果好、操作过程简便高效、灵敏度高、稳定性好和通用性强等优点,适用于花生中4种农药残留的同时检测。

       

      Abstract: A method was developed for simultaneous determination of the residues of quizalofop-p-ethyl, chlorpyrifos, acetochlor amd imidacloprid in peanut by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample was purified with a combination of Nano-ZrO2, C18 and multi-walled carbon nanotubes (MWCNT), detected by UPLC-MS/MS, and quantified by external standard method. The results showed that in the range of 0.001-0.5 mg/L, the linear relationship between the mass concentrations of the 4 pesticides and their corresponding peak areas was good, with r≥0.9986. At the three spike levels of 0.01, 0.1 and 1 mg/kg, the average recoveries of the four pesticides in peanuts were between 82% and 109%. And the relative standard deviations (RSDs, n = 5) were between 2.8% and 9.0%. Among them, the limit of quantification (LOQ) was 0.01 mg/kg. This method was used to test 10 batches of peanut samples collected from large supermarkets and agricultural markets in Tai’an City. The results showed that the residues of the four pesticides in all samples did not exceed the maximum residue limits set by China. This method has the advantages of good purification effect, simple and efficient operation, high sensitivity, good stability and strong versatility. It is suitable for the simultaneous detection of four pesticide residues in peanuts.

       

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