摘要
采用LC-MS法分离和鉴定盐酸西那卡塞有关物质。采用Hypersil C_(18)(100 mm×4.6 mm,2.4μm)色谱柱,以0.1%乙酸铵溶液-乙腈(93∶7)为流动相A相,乙腈为流动相B相进行线性梯度洗脱,对盐酸西那卡塞有关物质及强制降解产物进行分离。经过电喷雾正离子化-高分辨TOF/MS检测,同时结合MS/MS光谱和对照品对照,对各有关物质进行分析鉴定。在所建立的液-质联用分析条件下,盐酸西那卡塞及其有关物质得到有效的分离,共检测到10个有关物质,分别为盐酸西那卡塞合成起始原料(1个)、合成中间体(1个)、合成副产物(4个)和降解产物(5个)。建立的LC-MS法能有效鉴定盐酸西那卡塞有关物质,并为其质量控制和工艺优化研究提供参考依据。
To develop an LC-MS method for the separation and identification of the related substances in cinacalcet hydrochloride. The separation was carried out on a Thermo BDS Hypersil C18 column（100 mm×4. 6 mm, 2. 4 μm）with mobile phase consisting of 0. 1% ammonium acetate buffer-acetonitrile（93∶7）（A）and acetonitrile（B）by gradient elution. The related substances were identified by electrospray positive ionization high resolution TOF/MS and MS/MS, and verified further through reference substances. Cinacalcet hydrochloride and itsrelated substances were separated under the established LC-MS condition. Ten related substances were detected and identified to be one starting material, one intermediate, four synthetic by-products and five degradation products. It showed that the LC-MS method was useful for separating and identifying the related substances in cinacalcet hydrochloride. And the results obtained are valuable for cinacalcet hydrochloride manufacturing process control and quality assurance.
出处
《中国药科大学学报》
CAS
CSCD
北大核心
2016年第6期719-726,共8页
Journal of China Pharmaceutical University
