韩丙军, 何燕, 林冰, 黄海珠, 陈丽霞, 许丽建. 超高效液相色谱-串联质谱法测定甘蓝中三乙膦酸铝的残留[J]. 农药学学报, 2017, 19(3): 403-408. DOI: 10.16801/j.issn.1008-7303.2017.0053
    引用本文: 韩丙军, 何燕, 林冰, 黄海珠, 陈丽霞, 许丽建. 超高效液相色谱-串联质谱法测定甘蓝中三乙膦酸铝的残留[J]. 农药学学报, 2017, 19(3): 403-408. DOI: 10.16801/j.issn.1008-7303.2017.0053
    HAN Bingjun, HE Yan, LIN Bing, HUANG Haizhu, CHEN Lixia, XU Lijian. Determination of fosetyl-aluminium residue in cabbage (Brassica oleraceae L.) by using ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2017, 19(3): 403-408. DOI: 10.16801/j.issn.1008-7303.2017.0053
    Citation: HAN Bingjun, HE Yan, LIN Bing, HUANG Haizhu, CHEN Lixia, XU Lijian. Determination of fosetyl-aluminium residue in cabbage (Brassica oleraceae L.) by using ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2017, 19(3): 403-408. DOI: 10.16801/j.issn.1008-7303.2017.0053

    超高效液相色谱-串联质谱法测定甘蓝中三乙膦酸铝的残留

    Determination of fosetyl-aluminium residue in cabbage (Brassica oleraceae L.) by using ultra-high performance liquid chromatography-tandem mass spectrometry

    • 摘要: 建立了一种超高效液相色谱-串联质谱(UPLC-MS/MS)检测甘蓝中三乙膦酸铝残留的方法。通过测定甘蓝样品中乙基磷酸和亚磷酸的含量,对三乙膦酸铝进行定量。采用电喷雾负离子(ESI-)电离,多反应监测模式(MRM)定性分析,基质匹配标准曲线外标法定量。结果表明:三乙膦酸铝在不同配比的乙腈-水溶液中均可解离为乙基磷酸和亚磷酸,且二者的质量比均为40:60;三乙膦酸铝的检出限(LOD)为1.3 μg/kg;在10~500 μg/L范围内,乙基磷酸和亚磷酸的线性相关系数均大于0.999;在0.01、0.1和0.5 mg/kg 3个添加水平下,甘蓝中三乙膦酸铝的平均回收率在82%~107%之间,相对标准偏差(RSD)在6.7%~9.2%(n=5)之间。该方法简单、快速,灵敏度及准确度高,可满足甘蓝中三乙膦酸铝残留的检测要求。

       

      Abstract: A rapid method for analyzing the fosetyl-aluminium (Al) residues in Chinese cabbage was developed using ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). This method quantified the concentration of fosetyl-Al by determining the contents of ethyl phosphonic acid and phosphorous acid. Analytes were detected by electro-spray ionization (ESI-) and multiple reaction monitoring (MRM) mode. Fosetyl-Al dissociated as ethyl phosphonic acid and phosphoous acid, and the ratios between the two acids were 40:60 with different solution. Quantification was performed by peak area external standard methods using matrix-matched calibration curves, which were linear in the range of 10-500 μg/L with good linear relationships. The correlation coefficients were better than 0.999. The limit of quantification (LOQ) of fosetyl-Al was 1.3 μg/kg. At 0.01, 0.10 and 0.50 mg/kg spiked levels, the recoveries and the relative standard deviations (RSD) were 82%-107% and 6.7%-9.2% (n=5) for fosetyl-Al. This method was simple, rapid, accurate, which could be applied to the determination of fosetyl-Al residues in Chinese cabbage.

       

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