目的 对复方盐酸替利定口服液中的主要杂质进行归属性研究和结构确证。方法 采用HPLC,确定样品中的3个主要杂质均由盐酸替利定原料引入或降解;采用HPLC-MS联用方法对主要杂质进行结构推测,并通过柱色谱分离2个杂质,定向合成1个杂质,采用UV、IR、MS、NMR等测定方法对其进行综合结构解析。结果 确定了3个杂质的结构,杂质1为顺式替利定,杂质2为反式去甲基替利定,杂质3为顺式去甲基替利定。结论 3个杂质的结构确证对有关物质控制具有重要意义。

OBJECTIVE To explore the sources and structures of the main impurities in compound tilidine hydrochloride oral solution. METHODS The sample was shown by HPLC to have three major impurities originated from tilidine raw material or degradation of tilidine. The structures of the three major impurities were speculated by HPLC-MS, among which two were isolated by column chromatography and one was synthesized. The structures of the three impurities were elucidated with UV, IR, MS and NMR. RESULTS The molecular structures of three impurities of Compound Tilidine Hydrochloride Oral Solution were confirmed.mpurity one was the cis tilidine, Impurity two was the trans demethyltilidine. Impurity three was the cis demethyltilidine. CONCULSION The identification of three impurities have important significance for the control of the related substances.