HPLC测定注射用地西他滨的含量及有关物质

Determination of the Content of Decitabine for Injection and Its Related Substances by HPLC

关键词:  注射用地西他滨  含量测定  有关物质  高效液相色谱法

Key words:  decitabine for injection  content determination  related substance  HPLC

摘要:

目的 建立高效液相色谱法测定注射用地西他滨的含量及有关物质。方法 采用Shimpack VP-ODS色谱柱(250 mm×4.6 mm，5 μm)，以0.01 mol·L^-1磷酸钾缓冲液(用磷酸调节pH值至6.8)-甲醇(98∶2)为流动相，流速：1.0 mL·min^-1，检测波长：220 nm，柱温：15 ℃，进样量：5 μL。结果 主峰能与相邻杂质峰较好分离。地西他滨浓度在5.028~201.12 μg·mL^-1内与峰面积呈良好的线性关系，r=0.999 8。低、中、高浓度平均回收率(n=3)分别为99.8%，100.2%，99.6%；RSD分别为0.27%，0.51%，0.60%；测定3批样品的含量分别为100.6%，99.3%，99.5%，有关物质分别为0.56%，0.49%，0.44%。结论 该方法简便、准确、专属性强，可用于测定注射用地西他滨的含量及有关物质。

Abstract:

OBJECTIVE To establish an HPLC method to determine the content of decitabine for injection and its related substances. METHODS The assay was conducted on a Shimpack VP ODS column(250 mm×4.6 mm, 5 μm) with 0.01 mol·L^-1 solution of potassium phosphate buffer (adjust to pH 6.8 with phosphoric acid)-methanol (98∶2) as mobile phase at the flow rate of 1.0 mL·min^-1. The detection wavelength was set at 220 nm. Temperature was 15 ℃. The injection volume was 5 μL. RESULTS Decitabine was completely separated from impurities. The linear concentration range of decitabine was 5.028-201.12 μg·mL^-1 with the correlation coefficient of 0.999 8. The recoveries(n=3) of low, medium and high concentration were 99.8%, 100.2%, 99.6%, and RSDs were 0.27%, 0.51%, 0.60%, respectively. Determination of the content of three samples were 100.6%, 99.3%, 99.5%, the related substances were 0.56%, 0.49%, 0.44%. CONCLUSION The method is simple, accurate, specific and suitable for the determination of the content and the related substances of decitabine for injection.