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[目的]为研究不同生产工艺对农药2,4-滴产品中二噁英类含量的影响,采用同位素稀释高分辨气相色谱-高分辨质谱法(HRGC-HRMS)对2,3,7,8-氯代二噁英类进行定量分析。[方法]采用液液萃取法对2,4-滴产品进行提取,酸碱复合硅胶柱和活性炭硅胶柱进行净化,同位素稀释和气相色谱/高分辨磁质谱联用仪(GC/HRMS)分析等步骤,测定17个2,3,7,8-氯取代二噁英类化合物。[结果]由于强碱溶液对氯化后的中间体起到了抑制二噁英产生的作用,因此先氯化后缩合生产工艺的2,4-滴产品中二噁英含量较低。
[Objective] The research aimed to study the effect of different production processes on the dioxin content in 2,4-D products of pesticides. The isotope dilution high-resolution gas chromatography-high resolution mass spectrometry (HRGC-HRMS) - Chloro Dioxins for Quantitative Analysis. [Method] The 2,4-D products were extracted by liquid-liquid extraction method, and purified by acid-base silica gel column and activated carbon silica gel column, and analyzed by isotope dilution and gas chromatography / high resolution mass spectrometry (GC / HRMS) Step, measuring 17 2,3,7,8-chloro-substituted dioxins. [Result] The dioxin contents in the 2,4-drop products after the first chlorination and condensation production process were lower because the strong alkali solution played a role in inhibiting the production of dioxins after the chlorination.