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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 a HPLC method for the determination of rupatadine fumarate and related substances. Methods: The mobile phase was XTerra-C18 (250mm × 4.6mm, 5μm) with acetate buffer (pH 4.0) -methanol (25:75) as mobile phase at a flow rate of 1.0mL · min-1 and the detection wavelength was set at 244nm. The main related substances were identified by LC-MS / MS. Results: The substance was separated from rupatadine fumarate well and the concentration of rupatadine fumarate was linear (r = 1.000) in the range of 0.2 ~ 200μg.mL-1. The detection limit was 0.1μg.mL- 1; the main related substances in rupatadine fumarate are 3-dibromomethyl-5-methylpyridine, desloratadine, 3,5-bis (desloratadine) methyl Pyridine. Conclusion: This method is accurate and accurate and can be used for determination of rupatadine fumarate and related substances.