Uncertainty Evaluationon of the Content Determination of Cinacalcet Hydrochloride by HPLC / 中国药师

ABSTRACT

Objective:To establish an HPLC method for the content determination of cinacalcet hydrochloride and evaluate the un-certainty in the measurement. Methods:An Inertsil ODS-SP chromatographic column(250 mm×4.6 mm,5 μm) was used,the mo-bile phase was composed of phosphate buffer solution(pH 6.5) and acetonitrile(60 40),the flow rate was 1.0 ml·min-1,the de-tection wavelength was 272 nm,the column temperature was 30℃ and the injection volume was 20 μl. The content calculation formula-tion was deduced,the influencing factors were determined,and each component was assessed. Results:The resolution between cina-calcet and the impurity was satisfied,the linear relationship within the range of 10-100 μg?ml-1was excellent(r=0.999 9),the av-erage 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,ac-curate and reliable,and can provide reference for the development of quality standards for generic drugs. Based on the influencing fac-tors of uncertainty,the main influencing reasons for the determination results can be found out to improve the reliability of determina-tion.