RP-HPLC法测定PAC-1盐酸盐的含量及有关物质

目的建立RP-HPLC方法测定PAC-1盐酸盐含量并进行有关物质检查。方法采用KromasilC18色谱柱(150 mm×4.6 mm,5μm),流动相:乙腈-甲醇-磷酸盐缓冲液(30 mmo.lL-1磷酸二氢钾,体积分数为0.06%的磷酸溶液)(体积比为35∶5∶60),流速:1.0 mL.min-1,UV检测波长:281 nm,柱温:35℃。结果PAC-1盐酸盐在2.00~50.10 mg.L-1内线性关系良好(r=0.999 9),平均回收率为100.3%(RSD=0.8%)。PAC-1盐酸盐与其有关物质得到良好分离,检测限为0.2 ng。结论本方法可用作PAC-1盐酸盐含量测定和有关物质检查。

Determination of PAC-1 hydrochloride and its related substances by RP-HPLC

Objective To establish an HPLC method for determining the content of PAC-1 hydrochloride and its related substances. Methods The determination of PAC-1 hydrochloride and the separation of its related substances was performed on a Kromasil C₁₈ column (150 mm × 4.6 mm , 5 μm).The mobile phase was acetonitrile-methanol-phosphate buffer solution (30 mmol&;#8226;L^-1 potassium dihydrogen phosphate, 0.06 % Phosphoric acid) (V:V=35:5:60).The flow rate was 1.0 mL&;#8226;min^-1. Ultraviolet absorption detector was set at 281 nm and column temperature at 35 ℃. Results The linear range of PAC-1 hydrochloride was between 2.00 and 50.10 µg&;#8226;mL^-1 (r = 0.999 9). The average recovery was 100.3 % with RSD of 0.8 %. The related substances of PAC^-1 hydrochloride could be completely separated from PAC-1 hydrochloride. The limit of detection (LOD) was 0.2 ng. Conclusion The method is simple and accurate for quality control of the PAC^-1 hydrochloride .