水蛭冻干粉针剂指纹图谱评价

Study on fingerprint of Leech Lyophilized Injection

目的:建立注射用水蛭冻干粉针剂指纹图谱,为其质量控制提供依据.方法:按照国家食品药品监督管理局(SFDA)颁布的"中药色谱指纹图谱相似度评价系统2004A版"评价指南和《中国药典》2005年版一部附录HPLC法,筛选有效和稳定的色谱柱、流动相、检测波长、供试品溶液配制等检测条件,对10批水蛭冻干粉针剂的指纹进行检测.结果:①高效液相色谱(HPLC)法检测条件为KromasilKR100-5C18色谱柱(250mm×4.6mm,5μm),水-甲醇-四氢呋喃(100∶0.1∶0.05)为流动相,检测波长249nm;次黄嘌呤对照品为参比物,分析各色谱峰与次黄嘌呤色谱峰的相对保留时间和相对峰面积值的相对标准偏差(RSD).②10批次水蛭冻干粉针剂HPLC分析发现主要由5个主峰构成其指纹特征.③10批次样品中次黄嘌呤色谱峰所对应的保留时间一致,各色谱峰与次黄嘌呤色谱峰的相对保留时间和相对峰面积RSD%均符合指纹图谱的检测要求,指纹图谱的相似度均大于0.92.结论:建立的检测水蛭冻干粉针剂指纹图谱HPLC方法,操作简便、结果准确、重现性好,可用于水蛭冻干粉针剂的质量监控.

AIM：To establish fingerprint of Leech Lyophilized Injection for quality control.METHODS：According to the evaluating system 2004A issued by State food and drug administration（SFDA）and appendix of Pharmacopoeia of People＇s Republic of China I,we filtered the Conditions as chromatographic column,mobilephase,determination wavelength,testing solution preparing and test the fingerprint of 10 patches of Leech Lyophilized Injection.RESULTS：① The high performance liquid chromatography（HPLC）method was set up using Kromasil KR100-5C18（250 mm×4.6 mm,5 μm）column with mobile phase of water-methanol-tetrahydrofuran（100∶0.1∶0.05）,and determination wavelength was 249 nm.In the recorded chromatogram of the test preparation,Relative Standard Deviation（RSD）of the relative retention time and the relative peak areas of all peaks compared with hypoxanthine peak were measured.The similarity of 10 patches of Leech Lyophilized Injection was appraised by the similarity evaluation system.② In this chromatogram condition,5 peaks were identified as the characteristic fingerprint of Leech Lyophilized Injection.③ The retention time for hypoxanthine in Leech Lyophilized Injection were consistent with each other.RSD（%）of the relative retention time and the relative peak areas of all peaks compared with hypoxanthine peak fit the requirements of fingerprint.The chromatography showed good similarity up to 92% in 10 patches of Leech LyophilizedInjection.CONCLUSION：The HPLC method of testing fingerprint of Leech Lyophilized Injection is exact,simple and accurate,and can be used for quality control of Leech Lyophilized Injection.