中药五味子中木脂素类成分的HPLC-MS研究及以中草药生物活性成分为基础的主成分聚类分析
摘要
中药是我国的文化瑰宝，在我国有着上千年的应用历史。中药中的中成药及独特的理论体系是中医药的精华所在。由于中药原料质量不稳定，疗效组分与作用机理不够明确，中成药生产工艺缺乏科学质量管理规范，严重影响了临床应用和发展。要解决这些难题，就必须实现中药的现代化。色谱—质谱联用技术能够在研究和解决中药面临的很多理论与关键技术问题中，发挥着重要的作用。
目前，应用色谱—质谱联用技术来研究中药进行得很多，主要包括一下几个方面。1、在中草药常规分析中的应用；2、在中药复方中的应用；3、在中药质量控制中的应用。而随着指纹图潜概念的提出，近年来应用HPLC-MS技术制定中药指纹图谱，进而实现对中药的现代化质量控制的研究工作越来越多。迄今，HPLC-MS技术已经发展成为中草药研究的主要工具之一。
本文应用HPLC及MS联用技术，对中药五味子及天然产物茶叶进行了分析测定、分离制备和质量评价的研究探索工作，成果理想，很有实际应用价值。
一、利用HPLC—MS分析五味子果实中的木脂素成分，提出了一种简单、快速的木脂素化合物常规分析方法，能够准确定性定量测定木脂素化合物，检测限达到0.1-0.5 ng ml~(-1)。
二、利用硅胶柱层析分离技术，对比选择合适的溶剂洗脱，经过高效液相制备色谱(Prep—HPLC)分离纯化，分离制备了五味子果实
中3种主要木脂素成分:五味子素(schisandrin)、去氧五味子素
(deoxyschisandrin)、Y一五味子素(Y一Sehisandrin)。纯度大于
98%。
三、以茶叶水提物中的生物碱及多酚类化合物为目标，以HPLC理
化数据为样本，利用主成分一聚类分析法，对21种不同产地、品种的
茶叶样品进行了聚类分析，样品按品种、产地、内在品质差异得以区
分。此方法可用于评价天然产物(药物)之间的品质差异，可用于中
药指纹图谱的建立和比较。
Chinese Traditional Medicines (TCM) have been widely used in China for thousands of years. However, many works still have to be done in the field of modernization and standardization of TCM. Research work using high performance liquid chromatographic separation combined with the mass spectrometric technique can play an important role in this field.
Following works have been carried out in this research:
Firstly, an high-performance liquid chromatographic method coupled with electrospray-mass spectrometric detection based on selected ion monitoring has been developed for the determination of 7 lignans in the fruits of Schisandra Chinensis Baill. in one run. This method can be used to qualitative and quantitative detemination of lignans in Schisandra.
Secondly, we have successfully separated schisandrin, deoxyschisandrin and y -schisandrin by silica gel column elution and prep-HPLC. The purity of resulted products was higher than 98%.
Thirdly, the principal composition cluster analysis (PCA) was applied to treat HPLC data of nine catechins and alkaloids in water extracts of tea. The content relationship of nine
compounds was set as chemical descriptors and the samples were distinguished according to their species and geographical origins. The method can be used to estimate the quality of
different raw Chinese Traditional Medicines and applied in the
quality control of the fingerprint chromatogram for Chinese
Traditional Medicines.
目前，应用色谱—质谱联用技术来研究中药进行得很多，主要包括一下几个方面。1、在中草药常规分析中的应用；2、在中药复方中的应用；3、在中药质量控制中的应用。而随着指纹图潜概念的提出，近年来应用HPLC-MS技术制定中药指纹图谱，进而实现对中药的现代化质量控制的研究工作越来越多。迄今，HPLC-MS技术已经发展成为中草药研究的主要工具之一。
本文应用HPLC及MS联用技术，对中药五味子及天然产物茶叶进行了分析测定、分离制备和质量评价的研究探索工作，成果理想，很有实际应用价值。
一、利用HPLC—MS分析五味子果实中的木脂素成分，提出了一种简单、快速的木脂素化合物常规分析方法，能够准确定性定量测定木脂素化合物，检测限达到0.1-0.5 ng ml~(-1)。
二、利用硅胶柱层析分离技术，对比选择合适的溶剂洗脱，经过高效液相制备色谱(Prep—HPLC)分离纯化，分离制备了五味子果实
中3种主要木脂素成分:五味子素(schisandrin)、去氧五味子素
(deoxyschisandrin)、Y一五味子素(Y一Sehisandrin)。纯度大于
98%。
三、以茶叶水提物中的生物碱及多酚类化合物为目标，以HPLC理
化数据为样本，利用主成分一聚类分析法，对21种不同产地、品种的
茶叶样品进行了聚类分析，样品按品种、产地、内在品质差异得以区
分。此方法可用于评价天然产物(药物)之间的品质差异，可用于中
药指纹图谱的建立和比较。
Chinese Traditional Medicines (TCM) have been widely used in China for thousands of years. However, many works still have to be done in the field of modernization and standardization of TCM. Research work using high performance liquid chromatographic separation combined with the mass spectrometric technique can play an important role in this field.
Following works have been carried out in this research:
Firstly, an high-performance liquid chromatographic method coupled with electrospray-mass spectrometric detection based on selected ion monitoring has been developed for the determination of 7 lignans in the fruits of Schisandra Chinensis Baill. in one run. This method can be used to qualitative and quantitative detemination of lignans in Schisandra.
Secondly, we have successfully separated schisandrin, deoxyschisandrin and y -schisandrin by silica gel column elution and prep-HPLC. The purity of resulted products was higher than 98%.
Thirdly, the principal composition cluster analysis (PCA) was applied to treat HPLC data of nine catechins and alkaloids in water extracts of tea. The content relationship of nine
compounds was set as chemical descriptors and the samples were distinguished according to their species and geographical origins. The method can be used to estimate the quality of
different raw Chinese Traditional Medicines and applied in the
quality control of the fingerprint chromatogram for Chinese
Traditional Medicines.
引文
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