RP-HPLC法测定替勃龙原料药有关物质及含量

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。

RP-HPLC determination of content and related substances of tibolone

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.