论文部分内容阅读
目的:建立普乐沙福原料药有关物质的反相离子对高效液相色谱法。方法:采用离子对反相高效液相色谱法分析,以对照品外标法定性和定量。采用沃特世Xbridge C_(18)色谱柱(250 mm×4.6 mm,5μm),流动相为pH2.0庚烷磺酸钠-乙腈(80∶20),流速1.0 ml·min~(-1),检测波长210 nm,柱温35℃,进样量10μl。结果:普乐沙福与相邻杂质之间的分离度均大于1.5;有关物质1、2、3的定量限分别为21、35、26 ng,且在各自的线性范围内线性关系良好(r≥0.999 0);平均回收率分别为99.7%,100.3%,101.2%,RSD分别为1.1%,0.8%,1.7%(n=9)。结论:该方法专属性强、准确度高,适用于普乐沙福原料药的质量控制。
Objective: To establish a reversed-phase ion-pair high performance liquid chromatography (HPLC) method for the related substances of Plenafort. Methods: Ion-pair reverse-phase high-performance liquid chromatography was used for the qualitative and quantitative analysis of reference standard. A Waters Xbridge C_ (18) column (250 mm × 4.6 mm, 5 μm) was used with a mobile phase of pH2.0 sodium heptane sulfonate-acetonitrile (80:20) at a flow rate of 1.0 ml · min -1 , Detection wavelength 210 nm, column temperature 35 ℃, injection volume 10μl. Results: The separation between PlenaSulfide and adjacent impurities was more than 1.5. The quantitative limits of related substances 1, 2 and 3 were 21, 35 and 26 ng, respectively, and their linearity was good (r ≥0.999 0). The average recoveries were 99.7%, 100.3% and 101.2%, respectively, with RSDs of 1.1%, 0.8% and 1.7%, respectively (n = 9). Conclusion: The method is highly specific and accurate, and is suitable for the quality control of Preacharf APIs.