辅料聚维酮K30对缬沙坦胶囊质量控制的影响

Impact of the excipient povidone K30 on drug quality control of valsartan capsules

目的:对缬沙坦胶囊有关物质检查中一未知物质(相对于缬沙坦峰保留时间的0.14倍)进行来源与结构确证,探讨该未知物质对缬沙坦胶囊质量的影响,为质量标准的修订提供依据。方法:有关物质检查采用Inertsil ODS-4色谱柱(250 mm×4.6mm,5μm),以乙腈-水-冰醋酸(500∶500∶1)为流动相,流速1.0 mL·min-1,检测波长225 nm。对检出的该未知物质,采用UPLC-MS、IR、1H-NMR及MALDI-TOF-MS等技术确证其来源与结构。结果:通过以上检测技术的相互佐证,证实其为辅料聚维酮K30(PVP K30)。结论:辅料PVP K30峰不应计入有关物质,应在质量标准中增加扣除辅料峰的说明,以消除其对有关物质检查结果判定的影响。

Objective： To confirm the origin and structure of the unknown substance,eluted at 0.14 fold of the relative retention time of valsartan peak （RRT=0.14）,which was detected in related substances test of valsartan capsules;to explore the influence of the unknown material on the quality of valsartan capsules,and to provide basis for the revision of the quality standards. Methods： The analysis was carried out on an Inertsil ODS-4 column（250 mm×4.6 mm,5μm）with a mobile phase of acetonitrile-water-glacial acetic acid（500： 500： 1）at a flow rate of 1 mL·min^-1.The detective wavelength was set at 225 nm.UPLC-MS,IR,^1H-NMR and MALDI-TOF-MS techniques were applied to confirm the origin and structure of the unknown substance. Results： The unknown substance was confirmed to be the excipient povidone K30（PVP K30）. Conclusion： The excipient PVP K30 peak is not to be counted as the related substance of valsartan capsules,and it should be specified to deduct the excipient peak in ChP 2010 to eliminate the influence on the result of determination.