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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 a RP-HPLC method for the determination of related substances and content of tibolone drug substance. Methods: The mobile phase was Promosil-C18 (250 mm × 4.6 mm, 5 μm) with methanol-acetonitrile-water (50:30:20) as mobile phase at a flow rate of 1.0 mL · min- At room temperature, injection volume 10μL. Results: The linear range of tibolone was in the range of 0.5-250.0 μg · mL-1 (r = 0.9999). The correlation of the two substances in the test samples was detected by the principal component self-control method. The linear range was 0.2-20.0 μg · ML-1 (r = 0.9994). The detection limit was 0.05μg · mL-1. The average recoveries (n = 3) of low, medium and high concentrations of tibolone were 99.7%, 99.9% and 99.9%, respectively. The RSDs were 0.2%, 0.2% and 0.1% respectively. Conclusion: The method is simple, sensitive and reproducible, the results are accurate and reliable, which can be used for the detection and analysis of related substances and content of tibolone APIs and quality control.