替格瑞洛原料药中有关物质的HPLC法测定

Determination of the Related Substances in Bulk Drug of Ticagrelor by HPLC

建立了高效液相色谱法测定替格瑞洛原料药中的有关物质。使用Agilent Zorbax SB-C18色谱柱,以1.0 mol/L磷酸二氢钠缓冲液(pH 3.0)∶乙腈(90∶10)为流动相A,1.0 mol/L磷酸二氢钠缓冲液(p H 3.0)∶乙腈(30∶70)为流动相B,梯度洗脱,检测波长242 nm。替格瑞洛及其各有关物质(A^K)分离完全。有关物质A、D、E、F、G、H、I、J和K在各自定量限浓度至1.5mg/ml范围内线性关系良好,有关物质B和C在各自定量限浓度至3.0mg/ml范围内线性关系良好;平均回收率为95.1%~108.0%,RSD为0.83%~4.54%。

An HPLC method was established for the determination of the related substances in bulk drug of ticagrelor. An Agilent Zorbax SB-C18 column was used, with the mobile phase A of sodium dihydrogen phosphate buffer （1.0 mol/L） ： acetonitrile （90 ： 10）, and mobile phase B of sodium dihydrogen phosphate buffer （1.0 mol/L） ： acetonitrile （30 ：70）, by gradient elution at the detection wavelength of 242 nm. The peaks of the related substances and ticagrelor could be separated well. The method was found to be linear in the ranges of their LOQs to 1.5 lag/ml for the related substances A, D, E, F, G, H, I, J and K, in the ranges of their LOQs to 3.0 μg/ml for related substances B and C. Their average recoveries were 95.1% - 108.0 %, with RSDs of 0.83 % -4.54 %.