A validated RP-HPLC method for quantitative determination of related impurities of cholic acid bulk drugs

Acta Chromatographicae

Ye Ruhan¹  Sheng Zhaojun² 

[1] New Fortune Environmental Protection Co. Ltd. Yamen Jiangmen, Jiangmen 529152;School of Chemical and Environmental Engineering, Wuyi University, Jiangmen 529020

关键词: Reversed-phase HPLC;    quality control;    bulk drugs;    cholic acid;   

DOI  :  10.1556/1326.2017.00250

学科分类：化学（综合）

来源: Akademiai Kiado Rt.

【 摘 要 】

An efficient and convenient reversed-phase high-performance liquid chromatography method has been developed and validated for the quantitative determination of cholic acid bulk drugs and their related impurities. Chromatographic separation was performed on a YMC-Pack ODS-AQ column (250 mm × 4.6 mm, S-5 μm, 12 nm), and the mobile phase consisted of acetonitrile, methanol, and diluted formic acid solution (pH 2.5) at a flow rate of 1.0 mL/min. The analytes were monitored using a refractive index detector at 30 °C, and the column temperature was 30 °C. Under the above chromatographic conditions, the method has good specificity and specified impurities can be effectively separated. The proposed method is found to have linearity in the 2.0–80.0 μg/mL concentration range with correlation coefficients of not less than 0.9999. The compounds analyzed in the solutions are stable for at least 7 days, and spike recoveries for all specified impurities range from 91.3% to 109.3% with relative standard deviations (RSDs) not more than 7.3%. The limit of detection and the limit of quantification for the analytes are 0.060 μg/mL and 2.0 μg/mL, respectively. The proposed method can be applied in the quality control assay of cholic acid bulk drugs, with the advantages of simplicity, accuracy, robustness, good selectivity, and high sensitivity.

【 授权许可】

Unknown