尤庆航, 彭湃, 宋雨桐, 方楠, 朱宗利, 侯新港, 梁爽, 逯忠斌, 曲彤, 侯志广. 高效液相色谱-串联质谱法检测仲丁灵在人参中的残留及消解动态[J]. 农药学学报, 2021, 23(4): 739-746. DOI: 10.16801/j.issn.1008-7303.2021.0082
    引用本文: 尤庆航, 彭湃, 宋雨桐, 方楠, 朱宗利, 侯新港, 梁爽, 逯忠斌, 曲彤, 侯志广. 高效液相色谱-串联质谱法检测仲丁灵在人参中的残留及消解动态[J]. 农药学学报, 2021, 23(4): 739-746. DOI: 10.16801/j.issn.1008-7303.2021.0082
    YOU Qinghang, PENG Pai, SONG Yutong, FANG Nan, ZHU Zongli, HOU Xingang, LIANG Shuang, LU Zhongbin, QU Tong, HOU Zhiguang. Residues and dissipation dynamics of butralin in ginseng by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2021, 23(4): 739-746. DOI: 10.16801/j.issn.1008-7303.2021.0082
    Citation: YOU Qinghang, PENG Pai, SONG Yutong, FANG Nan, ZHU Zongli, HOU Xingang, LIANG Shuang, LU Zhongbin, QU Tong, HOU Zhiguang. Residues and dissipation dynamics of butralin in ginseng by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2021, 23(4): 739-746. DOI: 10.16801/j.issn.1008-7303.2021.0082

    高效液相色谱-串联质谱法检测仲丁灵在人参中的残留及消解动态

    Residues and dissipation dynamics of butralin in ginseng by high performance liquid chromatography-tandem mass spectrometry

    • 摘要: 建立了高效液相色谱-串联质谱(HPLC-MS/MS)测定人参中仲丁灵残留的分析方法,并研究其在人参中的最终残留量与消解规律。样品经乙腈提取,NH2固相萃取柱净化,液相色谱-串联质谱仪检测,外标法定量。结果表明:在0.002~0.5 mg/L内,仲丁灵的质量浓度与对应的峰面积间线性关系良好,鲜人参和干人参在0.01、0.05和0.5 mg/kg,人参植株和人参土壤在0.01、0.05、0.5和10 mg/kg添加水平下,仲丁灵的回收率为93%~108%,相对标准偏差为0.60%~6.2%。仲丁灵在人参植株和土壤中的半衰期为10.81~18.91 d,在鲜人参、干人参、人参植株和人参土壤中的最终残留量分别为<LOQ~0.010、<LOQ~0.024、0.011~0.19和0.16~0.41 mg/kg。建议我国仲丁灵在人参中的最大残留限量(MRL)可暂定为0.05 mg/kg,48%仲丁灵乳油以制剂量3750 g/hm2 (有效成分1800 g/hm2)在人参出苗前于土壤表面喷雾施药1次,收获期人参安全。

       

      Abstract: A high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the determination of the residues of butralin in ginseng was established, and the dissipation dynamics and terminal residues of butralin in ginseng were investigated. The samples were extracted by acetonitrile, cleaned-up by NH2 solid phase extraction (SPE) cartridges, detected by liquid chromatography-tandem mass spectrometry, and quantified with external standard method. The results showed that in the range of 0.002-0.5 mg/L, there was a good linear relationship between the mass concentration of butralin and the corresponding peak area. The recoveries of butralin were 93%-108% and the relative standard deviations were 0.60%-6.2% at spiking levels of 0.01, 0.05 and 0.5 mg/kg for fresh ginseng and dried ginseng and at spiking levels of 0.01, 0.05, 0.5 and 10 mg/kg for ginseng plant and soil. The half-lives of butralin in ginseng plant and soil were 10.81-18.91 days, and the terminal residues of butralin in fresh ginseng, dried ginseng, ginseng plant, and ginseng soil were <LOQ-0.010 mg/kg, <LOQ-0.024 mg/kg, 0.011-0.19 mg/kg, and 0.16-0.41 mg/kg, respectively. It is suggested that the maximum residue limit (MRL) of butralin in ginseng could be tentatively set at 0.05 mg/kg, and the harvested ginseng was safe for consumption after the 48% butralin EC was sprayed on the soil surface once at dosage of 3750 g/hm2 (active ingredient of 1800 g/hm2) before the emergence of ginseng seedling.

       

    /

    返回文章
    返回