唐红霞, 黄佳庆, 孙强, 温广月, 董茂锋, 王伟民. QuEChERS-高效液相色谱-串联质谱法检测 氟吡菌胺及其代谢物和霜霉威在叶用 莴苣中的残留及消解动态[J]. 农药学学报, 2021, 23(2): 388-394. DOI: 10.16801/j.issn.1008-7303.2021.0026
    引用本文: 唐红霞, 黄佳庆, 孙强, 温广月, 董茂锋, 王伟民. QuEChERS-高效液相色谱-串联质谱法检测 氟吡菌胺及其代谢物和霜霉威在叶用 莴苣中的残留及消解动态[J]. 农药学学报, 2021, 23(2): 388-394. DOI: 10.16801/j.issn.1008-7303.2021.0026
    TANG Hongxia, HUANG Jiaqing, SUN Qiang, WEN Guangyue, DONG Maofeng, WANG Weimin. Residue and dissipation of fluopicolide, its metabolite and propamocarb in the leaf lettuce using a modified QuEChERS method and HPLC-MS/MS[J]. Chinese Journal of Pesticide Science, 2021, 23(2): 388-394. DOI: 10.16801/j.issn.1008-7303.2021.0026
    Citation: TANG Hongxia, HUANG Jiaqing, SUN Qiang, WEN Guangyue, DONG Maofeng, WANG Weimin. Residue and dissipation of fluopicolide, its metabolite and propamocarb in the leaf lettuce using a modified QuEChERS method and HPLC-MS/MS[J]. Chinese Journal of Pesticide Science, 2021, 23(2): 388-394. DOI: 10.16801/j.issn.1008-7303.2021.0026

    QuEChERS-高效液相色谱-串联质谱法检测 氟吡菌胺及其代谢物和霜霉威在叶用 莴苣中的残留及消解动态

    Residue and dissipation of fluopicolide, its metabolite and propamocarb in the leaf lettuce using a modified QuEChERS method and HPLC-MS/MS

    • 摘要: 样品通过改良的QuEChERS方法提取净化,建立了高效液相色谱-串联质谱检测叶用莴苣 Loctuca sativa L. var. ramosa Hort. 中氟吡菌胺及其代谢物2,6-二氯苯甲酰胺和霜霉威残留量的分析方法。样品经乙腈提取,多壁碳纳米管净化,基质匹配标准溶液外标法定量。结果显示:在0.005~1 mg/L范围内,目标化合物的质量浓度与对应的响应值间呈良好线性关系 (R2 ≥ 0.999)。在0.02、0.1、2和100 mg/kg添加水平下,3种化合物在叶用莴苣中的回收率在85%~106%之间,相对标准偏差在1.0%~18%(n = 5) 之间;3种化合物的定量限均为0.02 mg/kg。田间试验结果表明,当687.5 g/L氟菌 • 霜霉威悬浮剂以有效成分928.13 g/hm2施药3次、施药间隔期为7 d时,叶用莴苣中氟吡菌胺和霜霉威的消解动态均符合一级反应动力学方程,半衰期分别为3.9~4.2和4.8~4.9 d。末次施药后5 d和7 d时,氟吡菌胺和霜霉威在叶用莴苣中的残留量分别为3.45~8.51和9.05~31.1 mg/kg,而2,6-二氯苯甲酰胺的残留量均低于定量限 (0.02 mg/kg)。结合中国和国际食品法典委员会 (CAC) 的最大残留限量以及叶用莴苣的生长特点和消费习惯,推荐687.5 g/L氟菌 • 霜霉威悬浮剂在叶用莴苣上施用的安全间隔期为5 d。

       

      Abstract: A modified QuEChERS approach had been developed for simultaneous determination of fluopicolide, its metabolite 2,6-dichlorobenzamide and propamocarb in the leaf lettuce by HPLC-MS/MS. The samples were extracted by acetonitrile with multi-wall carbon nanotubes (MWCNTs) for purification. The quantitative analysis of the samples achieved using the external standard of the matrix solution. The validation results showed that, in the range of 0.005-1 mg/L, the response of the concentrations of the compounds and the instruments had good linear relationship (R2 ≥ 0.999). Satisfied recoveries (85%-106%) and relative standard deviations (1.0%-18%) were obtained when spiked with 0.02, 0.1, 2, and 100 mg/kg in the samples. The acceptable limits of quantitation were 0.02 mg/kg for all the three compounds. In the field experiments, after sprayed by 928.13 g a.i./hm2 for 3 times and with a spraying interval of 7 d, the dissipation of fluopicolide and propamocarb in the leaf lettuce were following with the first-order kinetics equation, and their half-lives were 3.9-4.2 d for fluopicolide and 4.8-4.9 d for propamocarb, respectively. When the sample intervals were 5 d and 7 d, the residues levels of fluopicolide and propamocarb in the leaf lettuce were 3.45-8.51 mg/kg and 9.05-31.1 mg/kg, respectively. In terms of 2,6-dichlorobenzamide, the residues were lower than 0.02 mg/kg. Based on the growth characteristics and consumption habits of leaf lettuce, and the MRLs of China and Codex Alimentarius Commission (CAC), 5 d was selected as the post-harvest interval.

       

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