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目的:建立替格瑞洛片中有关物质的检测方法。方法:采用高效液相色谱法,色谱柱:Hypersil BDS C_(18)柱(200 mm×4.6 mm,5μm);以水(用磷酸调p H至3.0)为流动相A,以乙腈为流动相B,进行梯度洗脱;流速:1.0 ml·min~(-1);检测波长:255nm;柱温:30℃;进样量:5μl。结果:替格瑞洛与相邻杂质E及各已知杂质之间的分离度均大于1.5;杂质A~H均在2.0~20.0μg·ml~(-1)浓度范围内线性关系良好(r>0.996 0);杂质A~H的平均回收率分别为99.8%,98.1%,96.5%,101.2%,99.3%,100.7%,102.1%,103.4%,RSD(n=9)分别为1.02%,0.88%,1.13%,0.56%,0.79%,1.11%,0.63%,1.39%。结论:该法准确可靠,可用于替格瑞洛片中有关物质的测定。
Objective: To establish a method for the determination of related substances in ticagrelor tablets. Methods: High performance liquid chromatography (HPLC) was used. The column was Hypersil BDS C 18 column (200 mm × 4.6 mm, 5 μm) B, gradient elution; flow rate: 1.0 ml · min -1; detection wavelength: 255nm; column temperature: 30 ℃; injection volume: 5μl. Results: The separation between ticagrelor and adjacent impurities E and each known impurity was more than 1.5. The impurity A ~ H showed a good linearity in the range of 2.0 ~ 20.0μg · ml ~ (-1) (r > 0.996 0). The average recoveries of impurities A ~ H were respectively 99.8%, 98.1%, 96.5%, 101.2%, 99.3%, 100.7%, 102.1%, 103.4% and RSD (n = 9) 0.88%, 1.13%, 0.56%, 0.79%, 1.11%, 0.63%, 1.39%. Conclusion: This method is accurate and reliable and can be used for the determination of related substances in ticagrelor tablets.