盐酸地芬尼多杂质烯化合物的制备及结构确证

Preparation and Structure Confirmation of Impurity Olefinic Compound in Difenidol Hydrochloride

目的建立杂质烯化合物的制备方法并对其进行结构确证。方法采用盐酸地芬尼多原料经酸化、提取得到结晶,并经红外光谱、紫外光谱、液相色谱、质谱等方法确证其结构。结果制备的结晶经结构确证为杂质烯化合物,峰纯度为99.99%。结论该方法操作简便、专属性强、灵敏度高,制备的烯化合物结晶可用于盐酸地芬尼多原料及制剂有关物质检查中杂质烯化合物的定量测定。

Objective To establish a preparation method of impurity olefinic compound and to conduct the structure confirma- tion. Methods The raw material difenidol hydrochloride was adopted to obtain the crytal by aeidization and abstraction,and its structure was confirmed by the infrared spectra（IR）,ultravoilet（UV）, HPLC and MS methods. Results The prepared crytal structure was con- firmed to be the impurity olefinic compound. The peak purity was 99.99%. Conclusion This method is simple to operate ,strongly spe- cific and highly sensitive, and the prepared olefinic compound crytal can be used for the quantitative determination of impurity olefinic compound in the related substances of difenidol hydrochloride raw material and preparations.