芫花与黄芫花特征图谱以及主要化学成分含量的比较研究

Comparative study on the characteristic fingerprints and major chemical components between Flos Genkwa and Flos Wikstroemiae Chamaedaphnis

目的:建立芫花和黄芫花的特征图谱,并对芫花和黄芫花中主要化学成分进行定量研究。方法:采用HPLC-UV法建立芫花和黄芫花的特征图谱,采用Diamonsil C_(18)色谱柱(4.6 mm×250 mm,5μm),以乙腈(A)-0.1%甲酸水(B)为流动相,梯度洗脱,流速0.7 m L·min^(-1),检测波长350 nm,进样量20μL。采用LC-MS/MS法同时测定不同产地芫花和黄芫花中的主要化学成分含量,使用Agilent Zorbax SB C_(18)柱(150 mm×4.6 mm,5μm)色谱柱,流动相为甲醇(A)-0.1%甲酸水(B),梯度洗脱,流速0.8 m L·min^(-1),进样量10μL,以电喷雾离子源进行负离子模式扫描,多反应离子监测(MRM)进行定量分析。结果:采用HPLC-UV法分别建立了不同产地芫花和黄芫花药材的特征图谱,其中标定了6个共有峰作为芫花药材的特征峰,4个共有峰作为黄芫花药材的特征峰。采用HPLC-MS法同时测定了不同产地的11批芫花与16批黄芫花中的13种黄酮和3种酚酸类成分的含量,含量分析和聚类分析结果都表明芫花和黄芫花2种药材中主要成分存在显著性差异。结论:该法为芫花和黄芫花的鉴别和质量控制提供了科学依据,为临床用药的安全性提供了保障。

Objective：To establish the characteristic fingerprints of Flos Genkwa and Flos Wikstroemiae Chamaedaphnis,and simultaneously perform quantitative analysis of major chemical components in Flos Genkwa and Flos Wikstroemiae Chamaedaphnis.Methods：HPLC-UV was used to establish the characteristic fingerprints.The analysis was performed on a Diamonsil C_（18） chromatographic column（4.6 mm×250 mm,5 μm）.The mobile phase for gradient elution was acetonitrile（A） and 0.1% formic acid（B）;the flow rate was 0.7 m L·min-（-1）;the detection wavelength was set at 350 nm,and the injection volume was 20 μL.Quantitative analysis of major chemical components of Flos Genkwa and Flos Wikstroemiae Chamaedaphnis from different regions was performed on LC-MS/MS.Chromatographic separation was performed on an Agilent Zorbax SB C18 column（150 mm×4.6 mm,5 μm）eluted with methanol（A） and 0.1% formic acid（B） in a gradient elution at a flow rate of 0.8 m L·min^-1,and the injection volume was 10 μL. Electrospray ionization（ESI） in the negative ion mode and multiple-reaction monitoring（MRM） were applied for quantitative analysis.Results：The characteristic fingerprints of Flos Genkwa and Flos Wikstroemiae Chamaedaphnis were generated by HPLC-UV.There were six characteristic peaks for Flos Genkwa and four characteristic peaks for Flos Wikstroemiae Chamaedaphnis.The contents of 13 kinds of flavonoids and 3 kinds of phenolic acids in 11 bathces of Flos Genkwa and 16 batches of Flos Wikstroemiae Chamaedaphnis were determined by HPLC-MS.The results of quantitative analysis and clustering analysis showed that there were significant differences in the main components between Flos Genkwa and Flos Wikstroemiae Chamaedaphnis.Conclusion：The established method can provide the scientific basis for the identification and quality control of Flos Genkwa and Flos Wikstroemiae Chamaedaphnis,and guarantee the safety of clinical medication.