张鸿超, 陈德勇, 韩莹, 陈捷胤, 戴小枫, 孔志强, 颜廷才. QuEChERS-超高效液相色谱-串联质谱法测定6种典型农药及3种代谢物在黄瓜中的残留消解动态[J]. 农药学学报, 2022, 24(1): 168-176. DOI: 10.16801/j.issn.1008-7303.2021.0126
    引用本文: 张鸿超, 陈德勇, 韩莹, 陈捷胤, 戴小枫, 孔志强, 颜廷才. QuEChERS-超高效液相色谱-串联质谱法测定6种典型农药及3种代谢物在黄瓜中的残留消解动态[J]. 农药学学报, 2022, 24(1): 168-176. DOI: 10.16801/j.issn.1008-7303.2021.0126
    ZHANG Hongchao, CHEN Deyong, HAN Ying, CHEN Jieyin, DAI Xiaofeng, KONG Zhiqiang, YAN Tingcai. Residues and dissipation dynamics of six typical pesticides and three metabolites in cucumber by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2022, 24(1): 168-176. DOI: 10.16801/j.issn.1008-7303.2021.0126
    Citation: ZHANG Hongchao, CHEN Deyong, HAN Ying, CHEN Jieyin, DAI Xiaofeng, KONG Zhiqiang, YAN Tingcai. Residues and dissipation dynamics of six typical pesticides and three metabolites in cucumber by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2022, 24(1): 168-176. DOI: 10.16801/j.issn.1008-7303.2021.0126

    QuEChERS-超高效液相色谱-串联质谱法测定6种典型农药及3种代谢物在黄瓜中的残留消解动态

    Residues and dissipation dynamics of six typical pesticides and three metabolites in cucumber by QuEChERS-ultra 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) 同时检测黄瓜中多效唑、戊唑醇、丙硫菌唑、苯醚甲环唑、三唑酮、丁氟螨酯及3种代谢物B-3、三唑醇和CGA205375残留的分析方法,并采用该方法研究了6种农药不同施药剂量下在黄瓜中的消解动态。样品前处理采用QuEChERS方法,经乙腈提取,以N-丙基乙二胺 (PSA) 和石墨化碳黑 (GCB) 组合进行净化,采用UPLC-MS/MS检测,外标法定量。结果表明:在0.001~0.8 mg/L范围内,目标分析物的质量浓度与其对应的峰面积间线性关系良好,R2 > 0.9949;在0.001、0.01、0.05、0.1和0.5 mg/kg 5个添加水平下,6种农药及3种代谢物在黄瓜中的平均回收率在71%~105%之间,相对标准偏差 (RSDs,n = 5) 在1.7%~8.8%之间,其定量限 (LOQ) 在0.001~0.01 mg/kg之间。该方法净化效果好、操作简便高效、灵敏度高,可用于6种农药及3种代谢物残留的同时检测。田间试验采用6种农药按推荐剂量和5倍推荐剂量分别于黄瓜挂果期混合施药并进行采样检测。结果显示:除丙硫菌唑外,其余5种农药的消解动态均符合一级反应动力学方程,半衰期在3.15~9.62 d之间。研究结果可为上述农药的科学合理使用及其风险评估等提供参考。

       

      Abstract: A method for simultaneous determination of paclobutrazol, tebuconazole, prothioconazole, difenoconazole, triadimefon, cyflumetofen, and their metabolites including B-3, triadimend, CGA205375 residues in cucumber by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. This method was used to study the dissipation dynamics of six pesticides in cucumber at different dosages. QuEChERS method was employed for the sample preparation. The samples were extracted with acetonitrile, cleaned up with a combination of N-propyl ethylenediamine (PSA) and graphitized carbon black (GCB), detected by UPLC-MS/MS, and quantified by external standard method. The results showed that: in the range of 0.001-0.8 mg/L, the linear relationship between the mass concentration of the target analyte and its corresponding peak area was good with R2 > 0.9949; at the spiking levels of 0.001, 0.01, 0.05, 0.1 and 0.5 mg/kg, the average recoveries of six pesticides and their metabolites in cucumber were 71%-105%, the relative standard deviations (RSDs, n = 5) were 1.7%-8.8%, and the limit of quantification (LOQ) was 0.001-0.01 mg/kg. The method has the advantages of good cleanup efficiency, simple and efficient operation, and high sensitivity, and it can be applied to the simultaneous detection of the six pesticides and three metabolites in cucumber. In the field trials, both the recommended dose and five times of the recommended dose of the six pesticides were applied during the fruit-bearing period of cucumbers. The dissipation dynamics of five pesticides (except for prothioconazole) in cucumber all conformed to the first-order reaction kinetic equation, and the half-lives were 3.15-9.62 d. The research results provide references for the scientific and rational use of pesticides and their risk assessment.

       

    /

    返回文章
    返回