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目的建立高效液相色谱法测定盐酸普拉格雷原料药中有关物质。方法采用色谱柱为Cosmosil C18(250 mm×4.6 mm,5μm)柱;流动相为乙腈-磷酸盐缓冲溶液(p H值3.0,体积比为60∶40);流速为1.0 m L·min~(-1);检测波长为219 nm;进样量为10μL;柱温为30℃。结果杂质OHTP、杂质PFTP、杂质MFTP、杂质二酮、杂质OXTP、杂质CATP和盐酸普拉格雷的定量限分别为6.0×10-2、0.24、0.24、0.50、0.24、0.51和0.12 mg·L~(-1);检测限分别为20、80、80、170、80、170和40μg·L~(-1)。各杂质在考察的质量浓度范围内线性关系良好(r≥0.999 0),平均回收率分别为96.4%、97.7%、95.3%、96.7%、95.4%和95.4%(n=9)。结论该方法可用于盐酸普拉格雷有关物质的测定。
OBJECTIVE To establish a HPLC method for the determination of related substances in the raw material of prasugrel hydrochloride. Methods The column was Cosmosil C18 (250 mm × 4.6 mm, 5 μm). The mobile phase consisted of acetonitrile-phosphate buffer solution (p H value 3.0, volume ratio 60:40). The flow rate was 1.0 m L · min ~ -1). The detection wavelength was 219 nm. The injection volume was 10 μL. The column temperature was 30 ℃. Results The quantitative limits of impurity OHTP, impurity PFTP, impurity MFTP, impurity dione, impurity OXTP, impurity CATP and prasugrel hydrochloride were 6.0 × 10-2,0.24,0.24,0.50,0.24,0.51 and 0.12 mg · L ~ (-1). The detection limits were 20, 80, 80, 170, 80, 170 and 40 μg · L -1, respectively. Each impurity had a good linear relationship (r≥0.999 0) within the range of mass concentration examined. The average recoveries were 96.4%, 97.7%, 95.3%, 96.7%, 95.4% and 95.4% (n = 9), respectively. Conclusion This method can be used for the determination of related substances of prasugrel hydrochloride.