摘要
目的:建立HPLC法测定盐酸西那卡塞的含量,并进行不确定度评定。方法:采用Inertsil ODS-SP(250 mm×4.6 mm,5μm)为色谱柱,以磷酸盐缓冲液(pH 6.5)-乙腈(60∶40)为流动相,流速为1.0 ml·min^(-1),检测波长为272 nm,柱温为30℃,进样量为20μl;建立计算含量的数学模型,找出影响不确定度的因素,并对各个分量进行评估。结果:西那卡塞与各杂质之间分离良好,在10~100μg·ml^(-1)浓度范围线性关系良好(r=0.999 9),平均回收率为101.09%,RSD为0.54%(n=9),定量限(LOQ)为0.254μg·ml^(-1);盐酸西那卡塞含量扩展不确定度为1.22%,测量结果表示为(100.74±1.22)%(k=2)。结论:建立的高效液相色谱法操作简便、快捷、专属性好、结果准确、可靠,可为仿制药制定质量标准提供技术指导;通过分析影响不确定度的因素,找出影响检测结果的主要原因,提高检测结果的可信度。
Objective： To establish an HPLC method for the content determination of cinacalcet hydrochloride and evaluate the uncertainty in the measurement. Methods： An Inertsil ODS-SP chromatographic column（ 250 mm × 4. 6 mm,5 μm） was used,the mobile phase was composed of phosphate buffer solution（ pH 6. 5） and acetonitrile（ 60∶ 40）,the flow rate was 1. 0 ml·min^（-1）,the detection wavelength was 272 nm,the column temperature was 30℃ and the injection volume was 20 μl. The content calculation formulation was deduced,the influencing factors were determined,and each component was assessed. Results： The resolution between cinacalcet and the impurity was satisfied,the linear relationship within the range of 10-100 μg·ml^（-1） was excellent（ r = 0. 999 9）,the average recovery was 101. 09%（ RSD = 0. 54%,n = 9）,and the LOQ was 0. 254 μg·ml^（-1）. The expanded uncertainty was 1. 22%,and the result of the content determination was（ 100. 74 ± 1. 22） %（ k = 2）. Conclusion： The method is simple,fast,selective,accurate and reliable,and can provide reference for the development of quality standards for generic drugs. Based on the influencing factors of uncertainty,the main influencing reasons for the determination results can be found out to improve the reliability of determination.
出处
《中国药师》
CAS
2018年第2期368-371,共4页
China Pharmacist
