霍志铭, 李夏, 周昌敏, 何兆桓, 李国良, 姚丽贤. 1,2-苯二硫酚衍生-高效液相色谱法检测二硫代氨基甲酸酯类化合物的方法改进[J]. 农药学学报, 2015, 17(1): 68-74. DOI: 10.3969/j.issn.1008-7303.2015.01.09
    引用本文: 霍志铭, 李夏, 周昌敏, 何兆桓, 李国良, 姚丽贤. 1,2-苯二硫酚衍生-高效液相色谱法检测二硫代氨基甲酸酯类化合物的方法改进[J]. 农药学学报, 2015, 17(1): 68-74. DOI: 10.3969/j.issn.1008-7303.2015.01.09
    Huo Zhiming, Li Xia, Zhou Changmin, He Zhaohuan, Li Guoliang, Yao Lixian. Improvement on analysis of ethylenebisdithiocarbamate fungicide by 1,2-benzenedithiol derivatization-HPLC method[J]. Chinese Journal of Pesticide Science, 2015, 17(1): 68-74. DOI: 10.3969/j.issn.1008-7303.2015.01.09
    Citation: Huo Zhiming, Li Xia, Zhou Changmin, He Zhaohuan, Li Guoliang, Yao Lixian. Improvement on analysis of ethylenebisdithiocarbamate fungicide by 1,2-benzenedithiol derivatization-HPLC method[J]. Chinese Journal of Pesticide Science, 2015, 17(1): 68-74. DOI: 10.3969/j.issn.1008-7303.2015.01.09

    1,2-苯二硫酚衍生-高效液相色谱法检测二硫代氨基甲酸酯类化合物的方法改进

    Improvement on analysis of ethylenebisdithiocarbamate fungicide by 1,2-benzenedithiol derivatization-HPLC method

    • 摘要: 通过添加抗氧化剂四氢呋喃和抗坏血酸,对传统的二硫代氨基甲酸酯类化合物检测方法——1,2-苯二硫酚衍生-高效液相色谱法进行了优化和改进,并用4种常用二硫代氨基甲酸酯类杀菌剂70%代森锰锌可湿性粉剂(WP)、68% 精甲霜锰锌水分散粒剂(WG)、68%霜脲锰锌WG和55%唑醚代森联WG对该方法进行了验证。结果表明:当1,2-苯二硫酚浓度为12 mmol/L、代森锰锌用乙二胺四乙酸二钠(EDTA,pH 9.3)及代森联用二乙基三胺五乙酸(DTPA,pH 10.0)解络合、且同时添加体积分数为4%的四氢呋喃和40 mg/L的抗坏血酸时衍生化条件最优。除55%唑醚代森联WG 外,其他3种商品杀菌剂待测液在衍生化后48 h内均保持稳定且相对标准偏差<5%,满足测试要求。该方法操作简便快捷,检出目标物明确,不受二硫代氨基甲酸酯类杀菌剂常见代谢物乙撑硫脲及二硫化碳的影响,检测效率高,适用于该类杀菌剂的批量测试。

       

      Abstract: The traditional analysis of ethylenebisdithiocarbamate(EBDCs) fungicides by 1,2-benzenedithiol derivatization coupled with high performance liquid chromatography was improved by adding antioxidants vitamin C and THF to increase the stability of the reaction product. Four EBDCs fungicides including 70% mancozeb wettable power(WP), 68% metalaxyl-m mancozeb water dispersible granule(WG), 68% cymoxanil mancozeb WG and 55% pyraclostrobin metiram WG were used to validate this method. The results showed that the derivatization condition could be optimized by using 12 mmol/L 1,2-benzenedithiol, with EDTA(pH 9.3)/DTPA(pH 10.0) as decomplexants for mancozeb/metiram, simultaneously adding 4%(V:V) of tetrahydrofunan and vitamin C(40 mg/L). The determinants of EDBCs fungicides, with the exception of 55% pyraclostrobin metiram WG, were stable and quantificationally detectable with relative standard deviation less than 5% within 48 h. The improved method was demonstrated to be target-specific, inactive to EBDCs' metabolites like ethylenethiourea and CS2, and time-saving, which makes it practical for large-scale detection of EBDCs chemicals.

       

    /

    返回文章
    返回