RP-HPLC法测定富马酸卢帕他定含量及有关物质___

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(250 mm×46 mm，5 μm)柱，以醋酸盐缓冲液(pH 40)-甲醇(25∶75)为流动相，流速10 mL·min-1，检测波长244 nm。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2～200 μg·mL-1范围内线性良好(r=1000)；最低检测限为01 μg·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。

关键词：富马酸卢帕他定；含量测定；有关物质；反相高效液相色谱法

Abstract  Objective:To establish an RP-HPLC method for the determination of rupatadine fumarate and its related substances.Method:The separation was performed on a XTerra-C18(250 mm×46 mm,5 μm) 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.

Key words:rupatadine fumarate;determination;related substances;RP-HPLC