熊胆粉不同极性部位HPLC指纹图谱及化学模式识别研究  

HPLC fingerprint and chemical pattern recognition of different polar parts of Fel Ursi powder

作　　者：王晨曦 杨敏 梁红宝 姚景春 张贵民 冯帅[1] 李峰[1] WANG Chenxi;YANG Min;LIANG Hongbao;YAO Jingchun;ZHANG Guimin;FENG Shuai;LI Feng(School of Pharmacy,Shandong University of Traditional Chinese Medicine,Jinan 250355,China;State Key Laboratory of Integration and Innovation of Classic Formula and Modern Chinese Medicine,Lunan Pharmaceutical Group Co.,Ltd.,Linyi 276006,China)

机构地区：[1]山东中医药大学药学院,山东济南250355 [2]鲁南制药集团股份有限公司经方与现代中药融合创新全国重点实验室,山东临沂276006

出　　处：《中草药》2024年第3期770-779,共10页Chinese Traditional and Herbal Drugs

基　　金：山东省重大科技创新工程(2020CXGC010506);山东省自然科学基金项目(ZR2020KH018);2019泰山产业领军人才(tscy20200329)。

摘　　要：目的建立熊胆Fel Ursi粉不同极性部位的HPLC指纹图谱,比较不同提取部位化学成分之间的差异,为全面评价熊胆粉的质量评价提供参考。方法将熊胆粉分别用醋酸乙酯、三氯甲烷、丙酮、无水乙醇、乙腈依次提取,浓缩干燥,用甲醇溶解,建立HPLC指纹图谱,并采用相似度评价系统软件进行数据分析。结果10批熊胆粉醋酸乙酯部位共有模式共标记6个共有峰,三氯甲烷部位共有模式共标记8个共有峰,丙酮部位共有模式共标记8个共有峰,乙腈部位共有模式共标记10个共有峰,乙醇部位共有模式共标记16个共有峰,5种溶剂提取物均指认了4个共有指纹峰(牛磺熊去氧胆酸、牛磺鹅去氧胆酸、熊去氧胆酸、鹅去氧胆酸)。综合聚类分析和主成分分析(principal component analysis,PCA)结果,发现相同产地的熊胆粉,受不同厂家加工方法不同的影响,也存在一定的质量差异。通过正交偏最小二乘-判别分析(orthogonal partial least squares-discriminant analysis,OPLS-DA),发现牛磺熊去氧胆酸、牛磺鹅去氧胆酸、熊去氧胆酸、鹅去氧胆酸、乙醇部位10号峰、乙腈部位1、2号峰可能是熊胆粉质量差异的主要标志性成分。结论所建立的HPLC指纹图谱可以反映熊胆粉的化学成分分布,为熊胆粉的整体质量评价提供参考,并为熊胆粉谱效关系研究提供一定依据。Objective To establish the HPLC fingerprints of different polarity fractions from Xiongdan(Fel Ursi)powder and compare the differences of chemical composition between the different extractions from Fel Ursi powder,and provide a reference for comprehensive evaluation of the quality of Fel Ursi powder.Method Fel Ursi powder was extracted by ethyl acetate,chloroform,acetone,anhydrous ethanol and acetonitrile,concentrated and dried,dissolved with methanol to obtain samples.The samples were analyzed by HPLC fingerprints.The similarity evaluation software was used for data analysis.Results In 10 batches of Fel Ursi powder,a total of six common peaks were selected as the fingerprint peaks from the ethyl acetate extracts.A total of eight common peaks were identified from the HPLC fingerprint of chloroform extracts.A total of eight common peaks were identified from the acetone part of HPLC fingerprints.A total of 10 common peaks were identified from the HPLC fingerprint of acetonitrile extraction.A total of 16 common peaks were identified from the anhydrous ethanol extraction of HPLC fingerprints.A total of four common peaks(tauroursodeoxycholic acid,taurochenodeoxycholic acid,ursodeoxycholic acid,chenodeoxycholic acid)were identified from the five solvents.Based on the results of cluster analysis and principal component analysis(PCA),it was found that Fel Ursi powder from the same producing area also had certain quality differences due to the different processing methods of different manufacturers.Through orthogonal partial least squares-discriminant analysis(OPLS-DA),it was found that tauroursodeoxycholic acid,taurochenodeoxycholic acid,ursodeoxycholic acid,chenodeoxycholic acid,peak 10 of the ethanol fraction,peaks 1,2 of the acetonitrile fraction may be the main marker components of Fel Ursi powder quality differences.Conclusion The established HPLC fingerprints can fully reflect the distribution of the chemical composition of Fel Ursi powder,which provide reference for the quality evaluation of Fel Ursi powder,and pr

关 键 词：熊胆粉 极性部位 HPLC 指纹图谱 质量评价 化学模式识别 牛磺熊去氧胆酸 牛磺鹅去氧胆酸 熊去氧胆酸 鹅去氧胆酸 聚类分析 主成分分析 正交偏最小二乘-判别分析 

分 类 号：R283.6[医药卫生—中药学]