基于HPLC指纹图谱与UPLC-Q Exactive Focus MS/MS的黄芩炒炭前后化学成分变化  

Comparison of chemical compositions before and after charcoal-frying of Scutellariae Radix based on HPLC fingerprint and UPLC-Q Exactive Focus MS/MS

作　　者：李永康 曹立华 陈智[1] LI Yongkang;CAO Lihua;CHEN Zhi(College of Pharmacy,Shandong University of Traditional Chinese Medicine,Jinan 250355,China)

机构地区：[1]山东中医药大学药学院,山东济南250355

出　　处：《中草药》2024年第24期8425-8434,共10页Chinese Traditional and Herbal Drugs

基　　金：山东省自然科学基金面上项目(ZR2021MH009);山东省中医药科技项目(2021M143);山东中医药大学科学研究基金项目(KYZK2024M20)。

摘　　要：目的探究黄芩Scutellariae Radix炒炭前后的化学成分变化。方法HPLC法建立黄芩片及黄芩炭的指纹图谱,标定共有峰并通过主成分分析(principal component analysis,PCA)和正交偏最小二乘-判别分析(orthogonal partial least squares-discriminant analysis,OPLS-DA)筛选出黄芩炒炭前后的差异性成分。进一步通过UPLC-Q Exactive Focus MS/MS技术对差异性成分进行定性分析。结果建立的HPLC指纹图谱中,黄芩片标定了21个共有峰,15批黄芩片的相似度为0.998~1.000;黄芩炭标定了16个共有峰,15批黄芩炭的相似度为0.979~0.999;指认出黄芩炒炭前后28个差异性成分;通过UPLC-Q Exactive Focus MS/MS技术确定黄芩炭炮制前后的主要差异性成分为黄芩苷、汉黄芩苷、千层纸素A苷、黄芩素及汉黄芩素。结论通过对黄芩炒炭前后化学成分的系统研究,明确了黄芩炒炭前后的主要差异性成分,为完善黄芩片及黄芩炭质量标准提供了依据,为黄芩炭凉血止血谱效关系的研究提供了一定的参考依据。Objective To explore the changes of chemical composition of Huangqin(Scutellariae Radix,SR)before and after charcoal-frying.Methods The fingerprints of SR slices and charred SR were established by HPLC,the common peaks were indexed,and the differential components of SR before and after charcoal-frying were screened by principal component analysis(PCA)and orthogonal partial least squares-discriminant analysis(OPLS-DA).Qualitative analysis of differential components was performed using UPLC-Q Exactive Focus MS/MS technology.Results In the HPLC fingerprint,a total of 21 common peaks were demarcated in SR slices,and the similarity range of 15 batches of SR slices was 0.998-1.000,and a total of 16 common peaks were calibrated in charred SR,with a similarity range of 0.979-0.999,and 28 differential components were identified before and after charcoal-frying in SR.The primary differential components between SR and charred SR were determined to be baicalin,wogonoside,oroxyloside,baicalein,and wogonin,as identified through the use of UPLC-Q Exactive Focus MS/MS technology.Conclusion Through a systematic study of the chemical composition of SR before and after charcoal-frying,the major differential components between the two were identified.This research provided a basis for improving the quality standards of SR slices and charred SR,as well as offered certain reference for the study of the spectrum-effect relationship of charred SR for cooling blood and stopping bleeding.

关 键 词：黄芩片 黄芩炭 HPLC 指纹图谱 UPLC-Q Exactive Focus MS/MS 主成分分析 正交偏最小二乘-判别分析 黄芩苷 汉黄芩苷 千层纸素A苷 黄芩素 汉黄芩素 

分 类 号：R283.6[医药卫生—中药学]