摘要
目的:建立富马酸卢帕他定的HPLC含量测定及有关物质检查方法。方法:采用XTerra-C18(250mm×4.6mm,5μm)柱,以醋酸盐缓冲液(pH4.0)-甲醇(25∶75)为流动相,流速1.0mL·min-1,检测波长244nm。并采用LC-MS/MS法鉴定主要有关物质。结果:有关物质与富马酸卢帕他定分离良好,富马酸卢帕他定浓度在0.2～200μg.mL-1范围内线性良好(r=1.000);最低检测限为0.1μg.mL-1;富马酸卢帕他定中的主要有关物质分别为3-二溴甲基-5-甲基吡啶、地氯雷他定、3,5-二(地氯雷他定代)甲基吡啶。结论:本法专属准确,可用于富马酸卢帕他定的含量和有关物质测定。
Objective：To establish an RP -HPLC method for the determination of rupatadine fumarate and its related substances. Method：The separation was performed on a ）（Terra- C18 （250 mm×4. 6 mm,5μm） column,the mobile phase was composed of acetate buffer solution（pH 4. 0） -methanol（25： 75） ,and the flow rate was 1.0 mL·min^-1 with UV detection at 244 nm. LC - MS/MS method was employed for the identification of the major related substances. Results：Rupatadine fumarate and its related substances can be completely separated by the method with a good linear range of 0. 2 -200 μg·mL^-1 （r = 1. 000） and the LOD of 0. 1 μg·mL^-1.The related substances were characterized as 3 - dibromomethyl - 5 - methylpyridine ; desloratadine and 3,5 - di （ desloratadinyl ） methylpyridine. Conclusion： This RP - HPLC method is selective,accurate and suitable for the determination of rupatadine fumarate and its related substances.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2009年第5期791-794,共4页
Chinese Journal of Pharmaceutical Analysis
