厚朴炮制前后指纹图谱及主要成分含量变化的研究

Changes of HPLC Fingerprint and Main Contents of Magnolia Officinalis before and after Processing

目的:建立厚朴及其炮制品的HPLC指纹图谱,并对其所含的6个有效成分进行定量分析。方法:采用HPLC,Inertsil ODS-3 C18色谱柱(250 mm×4.6 mm,5μm),流动相乙腈-0.1%磷酸水溶液梯度洗脱,检测波长:250 nm,流速:1.0 ml·min^-1,建立生厚朴和姜厚朴的HPLC指纹图谱,通过相似度评价、聚类分析对厚朴炮制前后指纹图谱进行分析,并对紫丁香苷、木兰花碱、木兰苷B、木兰苷A、和厚朴酚与厚朴酚进行含量测定。结果:建立了厚朴及其炮制品的指纹图谱,以木兰苷B为参照峰,生厚朴标定了14个共有峰,姜厚朴标定了16个共有峰,与各自对照指纹图谱的相似度均>0.950。紫丁香苷、木兰花碱、木兰苷B、木兰苷A、和厚朴酚和厚朴酚在炮制前的质量分数分别为0.0423%,0.0614%,0.0815%,0.0881%,1.1900%,0.9690%;经炮制后,上述6种成分在姜厚朴中的含量分别为0.0346%,0.0331%,0.0657%,0.0705%,1.3300%,1.0900%。结论:厚朴的HPLC指纹图谱在炮制前后发生了显著变化,通过对比共有峰的保留时间和色谱图,指认出部分成分;并发现峰4和峰5为姜厚朴的特有峰,因此峰4和峰5可用于区别生厚朴和姜厚朴;6个有效成分含量在炮制前后均发生了一定程度的变化,样品中紫丁香苷、木兰花碱、木兰苷B和木兰苷A含量排序为厚朴>姜厚朴,样品中和厚朴酚和厚朴酚含量排序则为姜厚朴>厚朴。

Objective:To establish the HPLC fingerprints of Magnolia officinalis and its processed products,and to quantitatively analyze 6 components in Magnolia officinalis before and after processing.Methods:HPLC was employed with an Inertsil ODS-3 C18column(250 mm×4.6 mm,5μm),the mobile phase of acetonitrile-0.1%phosphoric acid aqueous solution was used with gradient elution,the detection wavelength was 250 nm,and the flow rate was 1.0 ml·min^-1.The HPLC fingerprints of the raw products and the processed products of Magnolia officinalis were established.Similarity evaluation and cluster analysis were used to analyze the chromatographic data.At the same time,the contents of syringin,magnoflorine,magnoloside B,magnoloside A,honokiol and magnolol were determined.Results:The HPLC fingerprints of Magnolia officinalis and its processed products were established.Taking magnoloside B as the reference peak,14 and 16 common peaks were demarcated for the raw products and its processed products,respectively,and the similarities of fingerprints were>0.950.The content of 6 components in the raw products were 0.0423%,0.0614%,0.0815%,0.0881%,1.19%and 0.969%,respectively.After processing,the content of the 6 components in the processed products was 0.0346%,0.0331%,0.0657%,0.0705%,1.3300%and 1.0900%,respectively.Conclusion:The HPLC fingerprint of Magnolia officinalis changes significantly after processing.Some components were identified by retention time and chromatogram of common peaks,and peak 4 and peak 5 were the characteristic peaks of the processed products,and can be used to distinguish the differences between the raw products and the processed products;the contents of 6 components change to a certain extent before and after processing.The content order of syringin,magnoflorine,magnoloside B and magnoloside A in the samples was raw products>processed products,while the content order of honokiol and magnolol was processed products>raw products.