薄层色谱法检查磷酸伯氨喹的有关物质及对映异构体的研究

Study on the Test for Related Substances of Primaquine Phosphate by TLC and Its Enantiomer

目的:建立磷酸伯氨喹的有关物质检查法及鉴定其对映异构体。方法:采用薄层色谱法常用的硅胶GF254薄层板,以醋酸乙酯-异丙醇-浓氨溶液(43∶35∶5)为展开剂,以自身对照法检查磷酸伯氨喹原料的有关物质。采用正相高效液相色谱法,以Waters5μm硅胶柱为色谱柱,检测波长为261nm,流动相为氯仿-正己烷-甲醇-浓氨溶液(45∶45∶10∶0.1),流速为2mL/min,确认其对映异构体。结果:有关物质均能达到较好分离,最低检出限可达0.3μg。薄层色谱中主斑点上方杂质斑点经鉴定为其对映异构体。结论:薄层色谱法较《英国药典》的高效液相色谱法更简便、快速,灵敏度较高,适用于磷酸伯氨喹的有关物质检查。

Objective:To establish a method of the test for related substances of primaquine phosphate and to authenticate its enantiomer. Methods:The related substances were tested by TLC,the coating substances was GF254,the mobile phase is a mixture of ethyl-isopropanol-concentrated ammonia solution(43 ∶35 ∶5)(V/V).The enantiomer was authenticated by HPLC using a column packed with silica gel (5 μm),the mobile phase is a mixture of chloroform-n-hexane-methanol-concentrated ammonia solution(45 ∶45 ∶10 ∶0.1)(V/V),UV detection was at 261 nm.Results:The related sabutances can be separated by TLC,the limit of test was 0.3 μg.The spot above the main spot was authenticated as its enantiomer.Conclusion:The method is simple,rapid and suitable for testing the related substances of primaquine phosphate.