多种色谱联用技术分析替曲朵辛

目的: 建立替曲朵辛原料药含量及有关物质的测定方法,并对有关物质的结构进行分析。 方法: 采用HPLC法测定替曲朵辛原料药含量及有关物质,采用UPLC-UV-MS/MS和LC-NMR联用技术对含量最高的杂质9的结构进行分析。 结果: 重复性好,替曲朵辛浓度在0.294~44.16 μg.mL^-1范围内线性关系良好(r＝0.9999),有关物质中最大杂质为4,9,10,11二脱水河豚毒素。 结论: 本方法操作简便,结果准确,可作为替曲朵辛原料药含量测定和有关物质检查的方法。

Objective: To establish a hyphenated chromatographic method for content determination of tetrodotoxin(TTX) raw medicine and related substances and to analyze the structure of related substances. Methods: HPLC was used to determin the content of tetrodotoxin raw medicine and related substances,and UPLC-UV-MS/MS and LC-NMR were used to study the structure of related substances. Results: There was a good linear relationship for tetrodotoxin in the range of 0.294-44.16 μg·mL^-1(r=0.9999).The impurity of the highest content was 4,9,10,11-dianhydro-TTX. Conclusion: The method is simple,accurate,and well reproducible which can be applied to content determination of Tetrodotoxin raw medicine and related substances.

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