基于指纹图谱分析和多成分同时定量的护肝片质量评价研究  

Quality evaluation of Hugan tablets based on HPLC fingerprint and simultaneous determination of multi-components

作　　者：杨瑾 殷智 袁德培 YANG Jin;YIN Zhi;YUAN De-pei(Medical School,Hubei University for Nationalities,Enshi 445000,China)

机构地区：[1]湖北民族学院医学院,恩施445000

出　　处：《药物分析杂志》2018年第11期2029-2037,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：生物资源保护与利用湖北省重点实验室开放基金项目(PKLHB171)

摘　　要：目的:建立护肝片的HPLC指纹图谱,并测定其主要成分的含量,为护肝片的质量控制提供可靠方法。方法:采用Agilent Zorbax SB-C_(18)色谱柱(250 mm×4.6 mm,5μm),以乙腈(A)-0.05%磷酸水溶液(B)为流动相,梯度洗脱(0～6 min,6%A;6～9 min,6%A→40%A;9～30 min,40%A→50%A;30～45 min,50%A;45～65 min,50%A→75%A),流速1.0 mL·min^(-1),检测波长250 nm,柱温30℃;建立护肝片HPLC指纹图谱,并对(R,S)-告依春、柴胡皂苷a、五味子醇甲、柴胡皂苷d、五味子酯甲、五味子甲素和五味子乙素的含量测定方法进行方法学考察。结果:在指纹图谱研究中,共确定护肝片HPLC指纹图谱20个共有峰,通过与混合对照品比较,指认其中7个指标成分,分别是(R,S)-告依春(1号峰)、柴胡皂苷a(3号峰)、五味子醇甲(5号峰)、柴胡皂苷d(6号峰)、五味子酯甲(8号峰)、五味子甲素(17号峰)和五味子乙素(20号峰),利用相似度软件对23批样品指纹图谱进行分析,各批样品相似度均在0.95以上。在建立的色谱条件下测定7个成分,分离度良好,方法精密度和重复性的RSD均<1.5%,供试品溶液在24 h内稳定,各成分具有良好的线性关系和较宽线性范围;6批护肝片中(R,S)-告依春、柴胡皂苷a、五味子醇甲、柴胡皂苷d、五味子酯甲、五味子甲素和五味子乙素质量分数分别为0.07～0.12、0.13～0.20、0.51～0.58、0.06～0.13、0.07～0.14、0.10～0.17和0.18～0.23 mg·片^(-1)。结论:所建立的护肝片HPLC指纹图谱检测和定量测定分析方法快速、准确,可以有效地评价护肝片的质量。Objective：To establish the HPLC fingerprint of Hugan tablets and determine the main components,so as to provide a reference for the quality control.Methods：The analysis was carried out on an Agilent Zorbax SB-C_（18） column（250 mm×4.6 mm,5 μm）with gradient elution of acetonitrile（A）-0.05% phosphoric acid aqueous solution（B）（0-6 min,6%A;6-9 min,6%A → 40%A;9-30 min,40%A → 50%A;30-45 min,50%A;45-65 min,50%A → 75%A）at a flow rate of 1.0 mL·min^（-1）. The detection wavelength was 250 nm and the column temperature was 30 ℃. The HPLC fingerprint was established,and determination method of（R,S）-epigoitrin,saikosaponin a,schisandrin,saikosaponin d,schisantherin,deoxyschizandrin and schisandrin B was studied methodologically. Results：20 common peaks were found in the fingerprint of Hugan tablets,7 of which were identified by comparison with the reference as（R,S）-epigoitrin（peak 1）,saikosaponin a（peak 3）,schisandrin（peak 5）,saikosaponin d（peak 6）,schisantherin（peak 8）,deoxyschizandrin（peak 17）and schisandrin B（peak 20）. The similarities of 23 batches of samples were above 0.95. The 7 compounds were well separated under the established chromatographic conditions. The RSD values for precision and repeatability tests were all less than 1.5% and the sample solution was stable during 24 h. All the compounds had a good linearity and wide linear range. The contents of（R,S）-epigoitrin,saikosaponin a,schisandrin,saikosaponin d,schisantherin,deoxyschizandrin and schisandrin B in 6 batches of Hugan tablets were 0.07-0.12 mg,0.13-0.20 mg,0.51-0.58 mg,0.06-0.13 mg,0.07-0.14 mg,0.10-0.17 mg tablet and 0.18-0.23 mg per tablet,respectively. Conclusion：The method is fast and accurate,and can be used for the quality control of Hugan tablets.

关 键 词：护肝片 高效液相色谱 (R S)-告依春 柴胡皂苷A 五味子醇甲 柴胡皂苷D 五味子酯甲 五味子甲素 五味子乙素 指纹图谱 质量控制 

分 类 号：R917[医药卫生—药物分析学]