戊酸雌二醇片有关物质检查及含量测定方法的研究

Determination of Content and Related Substances of Estradiol Valerate Tablets

目的:建立戊酸雌二醇片有关物质检查及含量测定的方法。方法:采用HPLC法,有关物质检查采用Waters NovaPack Phenyl柱(150 mm×3. 9 mm,4μm),以水-甲醇(60∶40)为流动相,流速为1. 0 ml·min^(-1),242 nm和280 nm双波长检测,柱温为室温,进样量为50μl。含量测定采用Hypersil BDS C_(18)柱(200 mm×4. 6 mm,5μm),以水-甲醇(15∶85)为流动相,流速为1. 0 ml·min^(-1),检测波长为280 nm,柱温为室温,进样量为20μl。结果:此条件下可分离9种以上戊酸雌二醇的有关物质。戊酸雌二醇在0. 939～391. 314μg·ml^(-1)范围内线性关系良好(r=0. 999 9),平均回收率为99. 68%(RSD=0. 48%,n=9)。结论:建立了有效的戊酸雌二醇片的质量控制方法,为戊酸雌二醇片质量标准收入国家标准提供有效的方法依据。

Objective: To establish a method to determine the content and related substances of estradiol valerate tablets. Methods: An HPLC method was used. For the determination of related substances,a Waters Nova-Pack Phenyl column (150 mm ×3. 9 mm,4 μm) was used,the mobile phase was water-methanol (60 ∶ 40),the flow rate was 1. 0 ml·min-1,the wavelengthes were242 nm and 280 nm,the column temperature was room temperature,and the injection volume was 50 μl. For the determination of content,a Hypersil BDS C18 column (200 mm × 4. 6 mm,5 μm) was used,the mobile phase was water-methanol (15 ∶ 85),the flow rate was 1. 0 ml·min-1,the detection wavelength was 280 nm,the column temperature was room temperature,and the injection volume was 20 μl. Results: More than 9 related substances of estradiol valerate were separated. Estradiol valerate showed a good linear relationship within the range of 0. 939-391. 314 μg·ml-1 (r = 0. 999 9) with the average recovery of 99. 68% (RSD = 0. 48%,n = 9).Conclusion: An effective method is established to control the quality of estradiol valerate tablets,which can provide technical basis for the quality research of estradiol valerate tablets.