RP-HPLC测定唑来膦酸含量及有关物质

Study on the assay of zoledronic acid and the determination of its related substances by RP-HPLC

目的 用反相离子对高效液相色谱法测定唑来膦酸的含量及有关物质。方法 采用DikmaC18(250mm×4.6 mm,5,μm)色谱柱,乙腈-离子对缓冲盐(取10％的四丁基氢氧化铵溶液6.0 mL,加水稀释至1000 mL,并用50％的磷酸溶液调节pH至2.3)(25:75)为流动相,检测波长为210 nm。结果 唑来膦酸有关物质与主成分的分离度及检出灵敏度完全达到要求,最小检出量为2 ng。浓度在32-480μg·mL-1内线性关系良好(r=1.000 0);平均回收率为100.2％,RSD为0.8％。结论本方法准确、简便、快速,能控制唑来膦酸及注射用唑来膦酸的质量。

OBJECTIVE: To establish an HPLC method for the assay of zoledronic acid and the determination of its related substances. METHOD: Dikma C18 column was used with acetonitrile-ion pair buffer solution (25:75) as the mobile phase. The buffer was prepared by dissolving 6.0 mL 10% tetrabutyl ammonium hydroxide in 1 000 mL water and adjusted to pH 2.3 with 50% phosphoric acid. The detection wavelength was at 210 nm. RESULTS: The resolution was acceptable. The detection limit was 2 ng. The linear range was 32-480 μg&middotmL -1 (r = 1.000 0). The average recovery was 100.2% (RSD = 0.8%). CONCLUSIONS: This method is simple, sensitive and accurate. It can be used to control the quality of zoledronic acid and zoledronic acid injection.