摘要
目的:建立复方醋酸甲地孕酮片有关物质测定方法。方法:采用LC-MS-UV联用技术对复方醋酸甲地孕酮片中最大杂质(杂质B)和次大杂质(杂质A)进行结构确证,并采用HPLC法对其定量,对其他杂质按自身对照法计算。采用Agela Vensuil XBP C18(L)色谱柱(4.6 mm×250 mm,5μm),流动相:乙腈-水(50∶50),流速:1.0 mL·min-1,检测波长:243 nm(杂质A、杂质B),291 nm(其他杂质),柱温:30℃,进样量:20μL。结果:杂质A和杂质B的浓度分别在0.308～10.28μg·mL-1和1.137～113.7μg·mL-1范围内线性关系良好,相关系数(n=5)均为1.000,平均回收率分别为101.9%和99.6%(n=9),RSD为0.83%和1.1%(n=3),最低检出限分别为0.5 ng和1.1 ng。结论:所建立的方法简便、快速,可准确测定该制剂中杂质含量。
To establish a method for the determination of the related substances of compound megestrol acetate tablets. Methods ： The structures of the maximum impurity （ impurity B ） and secondary maximum impurity （impurity A）were confirmed by LC - MS and the contents of the two impurities were quantified by HPLC. Other impurities were calculated by the main component self - contrasted method. An Agela Venusil XBP C18 （L） （4.6 mm × 250 mm, 5μm） was used with a mobile phase of acetonitrile - water （50： 50）. The flow rate was 1.0 mL · min-1 ,the detection wavelengths were 243 nm for impurity A and impurity B,and 291 nm for other impurities. The column temperature was 30 ℃, and the volume of injection was 20 μL. Results： Good linear correlations of impurity A and impurity B were observed within the ranges of 0. 308 - 10. 28 μg · mL-land 1. 137 - 113.7 μg · mL-1 （r = 1. 000） （ n = 5 ） ; the average recovery rates were 101.9% and 99.6% （ n = 9 ） , respectively. The RSDs were 0. 83% and 1.1% （n = 3）. The limits of detection were 0.5 ng and 1.1 ng, respectively. Conclusion：The method is simple,rapid, and accurate for determination of impurity content in preparation of compound megestrol acetate tablets.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2013年第11期1964-1970,共7页
Chinese Journal of Pharmaceutical Analysis
