摘要
目的:建立RP-HPLC法测定替勃龙原料药的有关物质及含量。方法:采用Promosil-C18柱(250 mm×4.6 mm,5μm),以甲醇-乙腈-水(50:30:20)为流动相,流速1.0 mL·min-1,检测波长204 nm,柱温为室温,进样量10μL。结果:替勃龙浓度在0.5～250.0μg·mL-1范围内呈良好的线性关系(r=0.9999);以主成分自身对照法检测供试品中的相关物质,线性范围是0.2～20.0μg·mL-1(r=0.9994);检出限为0.05μg·mL-1。替勃龙低、中、高浓度平均加样回收率(n=3)分别为99.7%,99.9%,99.9%;RSD分别为0.2%,0.2%,0.1%。结论:本方法简便、灵敏,重复性好,结果准确可靠,可用于替勃龙原料药有关物质及含量的检测与分析以及质量控制。
Objective：To establish an RP-HPLC method to determine the related substances of tibolone and its content.Method：The assay was conducted on a Promosil-C18 column（250 mm×4.6 mm,5 μm）with methanol-acetonitrile-water（50：30：20）as mobile phase at the flow rate of 1.0 mL·min-1,and the detection wavelength was 204 nm.The column temperature was room temperature and the injection volume was 10 μL.Results：The linear concentration range of tibolone was 0.5-250.0 μg·mL-1 with the correlation coefficient of 0.9999.It is detected the related substances with the method of the composition of the product itself,its linear concentration range was 0.2-20.0 μg·mL-1 with the coefficient of 0.9994,the detection limit was 0.05 μg·mL-1.The recoveries（n=3）of low,medium,and high concentration were 99.7%,99.9%,99.9%,and the RSDs were 0.2%,0.2%,0.1%,respectively.Conclusion：The method is simple,sensitive and reproducible,the results are accurate and reliable.It may be practical value for the quality control of tibolone and its related substances.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2012年第6期994-997,共4页
Chinese Journal of Pharmaceutical Analysis
基金
河北省科技攻关资助项目(05276101D-88)
河北教育厅科学研究计划项目(2009315)
河北省卫生厅医学科学研究重点课题计划项目(20090570)
河北省中医药管理局科研计划课题(2008072)
