王思威, 王潇楠, 常虹, 刘艳萍, 孙海滨. QuEChERS-高效液相色谱-串联质谱法检测荔枝中氯虫苯甲酰胺、溴氰虫酰胺及代谢物残留[J]. 农药学学报, 2022, 24(2): 395-403. DOI: 10.16801/j.issn.1008-7303.2021.0177
    引用本文: 王思威, 王潇楠, 常虹, 刘艳萍, 孙海滨. QuEChERS-高效液相色谱-串联质谱法检测荔枝中氯虫苯甲酰胺、溴氰虫酰胺及代谢物残留[J]. 农药学学报, 2022, 24(2): 395-403. DOI: 10.16801/j.issn.1008-7303.2021.0177
    WANG Siwei, WANG Xiaonan, CHANG Hong, LIU Yanping, SUN Haibin. Determination of chlorantraniliprole, cyantraniliprole and its metabolites residues in litchi using QuEChERS and high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2022, 24(2): 395-403. DOI: 10.16801/j.issn.1008-7303.2021.0177
    Citation: WANG Siwei, WANG Xiaonan, CHANG Hong, LIU Yanping, SUN Haibin. Determination of chlorantraniliprole, cyantraniliprole and its metabolites residues in litchi using QuEChERS and high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2022, 24(2): 395-403. DOI: 10.16801/j.issn.1008-7303.2021.0177

    QuEChERS-高效液相色谱-串联质谱法检测荔枝中氯虫苯甲酰胺、溴氰虫酰胺及代谢物残留

    Determination of chlorantraniliprole, cyantraniliprole and its metabolites residues in litchi using QuEChERS and high performance liquid chromatography-tandem mass spectrometry

    • 摘要: 采用高效液相色谱-串联质谱(HPLC-MS/MS)技术,结合改良的QuEChERS法,建立了同时测定荔枝中氯虫苯甲酰胺、溴氰虫酰胺及代谢物J9Z38残留的分析方法。样品用乙腈提取,以N-丙基乙二胺(PSA)和十八烷基键合硅胶(C18)组合吸附剂净化,采用C18反相色谱柱分离,以V(甲酸水溶液) : V(乙腈)=15 : 85为流动相,采用电喷雾正离子扫描(ESI+),多反应监测(MRM)模式,外标法定量。结果表明:3种目标化合物在0.005~1 mg/L范围内线性关系良好(r>0.99);方法的定量限(LOQs)为0.0005~0.01 mg/kg;在0.0005~0.5 mg/kg添加水平下,氯虫苯甲酰胺、溴氰虫酰胺及代谢物在荔枝全果和果肉中的平均回收率为76%~98%,相对标准偏差(RSD)为2.5%~9.6%。应用该方法对广州市场中的20批次荔枝样品进行检测,结果显示,氯虫苯甲酰胺检出量为0.001~0.01 mg/kg,溴氰虫酰胺及其代谢物J9Z38未检出。该方法简便、高效、快速,可用于荔枝样品中双酰胺类农药的同时检测。

       

      Abstract: An analytical method was established for simultaneous determination of chlorantraniliprole, cyantraniliprole and its metabolite J9Z38 in litchi by high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) combined with a modified QuEChERS procedure. The target compounds were extracted from the samples with acetonitrile and then cleaned up with primary secondary amine (PSA) and octadecylsilane (C18). The analytes were separated on a C18 column using V (formic acid aqueous solution) : V (acetonitrile)=15 : 85 as mobile phase and analyzed in multiple reaction monitoring (MRM) mode with positive electrospray ionization (ESI+). Quantitative analysis was performed by external standard method using matrix-matched calibration curves. The results showed that the linearity of the target compounds was good (r >0.99) in the range of 0.005-1 mg/L. The limits of quantification (LOQs) were 0.0005-0.01 mg/kg. The average recoveries of the three pesticides in litchi (whole fruit and pulp) ranged from 76% to 98% at the spiked levels of 0.0005-0.5 mg/kg, with the relative standard deviations of 2.5% to 9.6%. The method was applied for the detection of twenty commercial litchi samples in Guangzhou City. The results showed that the residues of chlorantraniliprole were 0.001-0.01 mg/kg, and neither cyantraniliprole nor its metabolite J9Z38 were found. The proposed method is convenient, effective and rapid, and is suitable for the simultaneous determination of chlorantraniliprole, cyantraniliprole and its metabolite in litchi.

       

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