RP-HPLC法测定替勃龙原料药有关物质及含量  

RP-HPLC determination of content and related substances of tibolone

作　　者：赵燕燕[1,2] 高茜[2] 李月秋[1] 韩媛媛[1] 刘丽艳[2] 孙汉文[2] 

机构地区：[1]河北大学医学实验中心,保定071000 [2]河北大学化学与环境科学学院,保定071002

出　　处：《药物分析杂志》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)

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.

关 键 词：高效液相色谱法 替勃龙 原料药 有关物质 含量测定 对照法 质量控制 

分 类 号：R917[医药卫生—药物分析学]