基于~1H-NMR指纹图谱的四批市售桑白皮药材质量分析

The quality analysis of four batches raw Mori Cortex materials based on ~1H-NMR fingerprint

目的采用核磁共振~1H-NMR指纹图谱技术,结合多元统计分析方法研究四种市售桑白皮药材与标准药材的化学成分差异性并评价其质量。方法以氘代甲醇-氘代重水(体积比1∶1)混合溶剂提取药材,在温度298 K,观测频率600.25 MHz条件下采集~1H-NMR谱,NMR数据经分段积分处理后,分别进行相似度分析、层序聚类分析和OPLS-DA分析。结果桑皮苷A、桑根皮醇、桑辛素、albanin A、grateloupinmaide、胆碱、蔗糖、乙酸、天门冬酰胺、葡萄糖、赖氨酸、氨基葡萄糖、精氨酸、丙氨酸、N-乙酰葡糖和柠檬酸是四种市售桑白皮药材与标准药材中有显著性差异的化学成分,桑皮苷A作为桑白皮的活性成分在四种市售药材中含量远低于标准药材,显示四种市售药材质量与标准药材存在较大差距。结论基于~1H-NMR和OPLS-DA的研究方法可以提供具体的差异性化学成分信息,并评价桑白皮药材的质量,为今后通过核磁共振技术建立桑白皮药材质量控制的方法提供参考和依据。

Objective To investigate the different chemical components between 4 batches of raw materials and standard of Moil Cortex using 1H-NMR fingerprint combined with multivariate statistical analysis. Methods ^1H-NMR spectra of the samples were acquired after ultrasonic extraction with mixture solvent [ V （CD3OD） ： V（D20） = 1：1 ] ,with the temperature at 298 K and spectrometer frequency of 600. 25 MHz. By using subsection integral method, the obtained NMR data was subjected to similarity analysis, hierarchical cluster analysis （ HCA ） and orthogonality partial least squares-discriminant, analysis （ OPLS-DA ）. Results Mulberroside A, morusinol, morusin, albanin A, grateloupinmaide, choline, sucrose, acetic acid, asparagines, glucose, lysine, glucosamine, arginine, alanine ,N-acetyl-D-glucosamine and citratewere identified as the main differential ingredients. Mulberroside A as the active ingredient of Mori Cortex, its contentin 4 batches of raw Mori Cortex materials was much lower than that in standard medicinal herb. Conclusions The method of ^1H- NMR combined with OPLS-DA can provide specific information about the difference on chemical composition, which provided contribution for the evaluation of Mori Cortex quality and provided reference and basis for the establishment of a quality control method for Mori Cortex in the future.