用HPLC指纹图谱对复方甘草片实施全质量控制研究  

Authentic quality control of compound liquoric tablets by HPLC fingerprints

作　　者：孙国祥[1] 智雪枝[1] 

机构地区：[1]沈阳药科大学药学院,沈阳110016

出　　处：《中南药学》2008年第3期349-355,共7页Central South Pharmacy

基　　金：国家自然科学基金重大研究计划项目(No.90612002)

摘　　要：目的采用双定性双定量相似度作为评价指标,建立了复方甘草片(CLTs)HPLC指纹图谱的全质量控制方法。方法采用RP-HPLC法以Century SIL C18BDS柱(200mm×4.6mm,5μm);以色谱指纹图谱相对指数Fr为指标优化选择指纹图谱检测条件,确定流动相为1%醋酸水-1%醋酸乙腈低压梯度洗脱,紫外检测波长:254nm,柱温:(30.00±0.15)℃,进样量:5μL。以双定性相似度为参量通过对21批CLTs进行系统聚类分析确定用其中13批CLTs对照指纹图谱(RFP),以此RFP为基础对总计26批CLTs采用双定性双定量相似度法进行质量评价。结果以甘草酸峰为参照物峰,确定35个指纹峰,建立了复方甘草片HPLC指纹图谱。用双定性双定量相似度法评价出11批质量完全合格,3批含量明显偏高,6批含量明显偏低,1批化学成分分布比例不合格,有劣质品(伪品)5批。结论所建立HPLC指纹图谱具有较好的精密度和重现性,适用于复方甘草片的质量控制。双定性双定量相似度法是宏观定性定量评价中药制剂质量的最合理、最客观的指纹图谱评价技术。Objective To establish an authentic quality control of compound liquoric tablets（CLTs）by HPLC fingerprints,using dual qualitative and dual quantitative similarities（DQDQS）as assessing parameters.Methods We used chromatographic fingerprint（CFP）relative index（Fr）to optimize the CFP conditions,and the CFPs were determined by injecting 5 μL of the sample solution each time on a CenturySIL C18 BDS column（200 mm×4.6 mm,5 μm）with the gradient elution solvent system composed of 1% acetate acid water and 1% acetate acid acetonitrile.The flow rate was 1 mL·min^-1,the column temperature was maintained at（30.00±0.15）℃ and the signals were acquired at 254 nm.The 21 batches of CLTs were identified with hierarchical clustering analysis using dual qualitative similarities as variables.According to the results of classification,the referential fingerprint（RFP）was synthesized from 13 batches of CLTs.With the RFP for the qualified model,a total of 26 batches of CLTs were evaluated by DQDQS.Results The CFPs containing 35 co-possessing peaks were obtained by choosing glycyrrhizic acid peak as the referential peak.Among the 26 batches of CLTs,11 were completely qualified,the contents of 3 batches were obviously higher while another 6 batches were lower,and the chemical constituents distributed proportion in 1 batch were not qualified and the rest 5 batches were inferior.Conclusion This new HPLC method with good precision and reproducibility can be applied in the quality control of CLTs.The DQDQS method is the most reasonable and an objective technique to assess and control the quality of Chinese traditional medicine preparations.

关 键 词：复方甘草片 HPLC指纹图谱 色谱指纹图谱相对指数Fr 双定性相似度 双定量相似度 系统聚类分析 

分 类 号：R927.11[医药卫生—药学] R284.11