宋雨桐, 陆洋, 尤庆航, 侯新港, 朱宗利, 孙晓伟, 方楠, 侯志广, 梁爽, 逯忠斌. 高效液相色谱-串联质谱法检测宁南霉素在人参中的残留及消解规律[J]. 农药学学报, 2021, 23(4): 747-753. DOI: 10.16801/j.issn.1008-7303.2021.0081
    引用本文: 宋雨桐, 陆洋, 尤庆航, 侯新港, 朱宗利, 孙晓伟, 方楠, 侯志广, 梁爽, 逯忠斌. 高效液相色谱-串联质谱法检测宁南霉素在人参中的残留及消解规律[J]. 农药学学报, 2021, 23(4): 747-753. DOI: 10.16801/j.issn.1008-7303.2021.0081
    SONG Yutong, LU Yang, YOU Qinghang, HOU Xingang, ZHU Zongli, SUN Xiaowei, FANG Nan, HOU Zhiguang, LIANG Shuang, LU Zhongbin. Residue and dissipation dynamics of ningnanmycin in ginseng by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2021, 23(4): 747-753. DOI: 10.16801/j.issn.1008-7303.2021.0081
    Citation: SONG Yutong, LU Yang, YOU Qinghang, HOU Xingang, ZHU Zongli, SUN Xiaowei, FANG Nan, HOU Zhiguang, LIANG Shuang, LU Zhongbin. Residue and dissipation dynamics of ningnanmycin in ginseng by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2021, 23(4): 747-753. DOI: 10.16801/j.issn.1008-7303.2021.0081

    高效液相色谱-串联质谱法检测宁南霉素在人参中的残留及消解规律

    Residue and dissipation dynamics of ningnanmycin in ginseng by high performance liquid chromatography-tandem mass spectrometry

    • 摘要: 为明确宁南霉素在人参上的消解规律和最终残留水平,于2019年在吉林省白山市、抚松县、延吉市以及辽宁省桓仁县4地进行了宁南霉素在人参及其植株中的田间残留及消解动态试验。样品经体积分数为0.2%的甲酸水溶液提取,采用PLS+PXC固相萃取柱净化,XSelect® HSS T3色谱柱分离,高效液相色谱-串联质谱 (HPLC-MS/MS) 测定。结果表明:在0.1、0.2和1 mg/kg添加水平下,宁南霉素在鲜人参和人参植株中的平均回收率分别为90%~99%和92%~94%,相对标准偏差 (RSD) 分别为4.7%~5.6%和4.0%~5.6%;在0.2、1和2 mg/kg添加水平下,宁南霉素在干人参中的平均回收率为89%~95%,RSD为1.4%~10%。在鲜人参与人参植株中的定量限 (LOQ) 均为 0.1 mg/kg,在干人参中的 LOQ 为 0.2 mg/kg。白山、桓仁两地的消解动态试验结果显示,宁南霉素在人参植株上的半衰期分别为11.77和0.76 d。4地的最终残留试验结果显示,宁南霉素在鲜人参上的最终残留量低于LOQ,在人参植株上的最终残留量为<LOQ~0.152 mg/kg,在干人参上的最终残留量低于LOQ。该结果表明,采用8%宁南霉素水剂防治人参疫病,按675~900 g/hm2 (有效成分54~72 g/hm2) 剂量施药3次,安全间隔期为14 d,收获期安全。

       

      Abstract: To investigate the dissipation and residues of ningnanmycin in ginseng, field trials of ningnanmycin residues in ginseng and its plants were conducted in Baishan City, Fusong County, Yanji City of Jilin Province, and Huanren County of Liaoning Province in 2019. The samples were extracted by 0.2% formic acid aqueous solution, cleaned up with PLS+PXC solid phase extraction column, separated by XSelect® HSS T3 column, and determined using HPLC-MS/MS. At 0.1, 0.2 and 1 mg/kg spiking levels, the average recoveries of ningnanmycin in fresh ginseng, ginseng plants were 90%-99%, 92%-94%, with the relative standard deviations (RSD) were 4.7%-5.6%, 4.0%-5.6%, respectively. At 0.2, 1 and 2 mg/kg spiking levels, the average recoveries of ningnanmycin in dried ginseng was 88%-95% with the RSD was 1.4%-10%. The limit of quantification (LOQ) of fresh ginseng and ginseng plants were both 0.1 mg/kg, and that of dried ginseng was 0.2 mg/kg. The results of the dissipation dynamic test in Baishan and Huanren showed that the half-lives of ningnanmycin on ginseng plants were 11.77 d and 0.76 d. The terminal residue results in 4 test places showed that the terminal residues of ningnanmycin on fresh ginseng, ginseng plants, and dried ginseng were <LOQ, <LOQ-0.152 mg/kg, and <LOQ, respectively. The results indicated that the harvested ginseng with the pre-harvest interval of 14 days would be safe for consumption after spraying 8% ningnanmycin AS at the recommended dosage of 675-900 g/hm2 (54-72 g a.i./hm2) 3 times to prevent and treat ginseng disease.

       

    /

    返回文章
    返回