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黄连素成分的原位薄层色谱-傅里叶变换-表面增强拉曼光谱研究

[In situ thin layer chromatography-fourier transform-surface-enhanced Raman spectrum study on ingredients of berberine].

作者信息

Wang Yuan, Guo Zhan-sheng, Wang Ying-feng, Wang Song-ying, Ren Gui-fen, Zhang Xiang-lan, Han Xiu-lan

机构信息

Chemisitry Department, Capital Normol University, Beijing 100037, China.

出版信息

Guang Pu Xue Yu Guang Pu Fen Xi. 2002 Oct;22(5):745-8.

Abstract

Surface Enhanced Raman Scattering (SERS) combined with Thin Layer Chromatography (TLC) has been used for studying characteristic spectrum of molecules in situ in micrograms samples. There are very few report for applying the SERS-TCL method in the study of the effective ingredients of Chinese traditional herbs. Coptis Chinensis France is an often-used clinic Chinese traditional medicine. Its main effective components include berberine and so on, which have antibiotic very wide and also have curative effect on improving the functions of heart vascular cycles. Therefore the concentrations of berberine are very important for the quality control of the medicine. In this work, the ethanol extract of Coptis Chinensis France was first separated by TLC, the SERS was then measure directly after dropping silver gel on the separated spots. The method can be used for the finger print analysis of the berberine. 3 microL of alcohol extract of Coptis Chinensis France with total alkaloids concentration of 1.0 mg.mL was placed on silicon GF254 TLC plate. The sample was separated by developing solvent of n bulanol-Acitic acid-H2O (7:2:1 V/V). The positions of berberine in the sample were confirmed by the standard alkaloid solutions. The Rf values for berberine are 0.29. The silver gel was used as surface enhanced substrate and placed on the separated berberine spots. FT-SERS was measured directly by a Nicolet FT-Raman 910 spectrometer. Berberine belong to isoquinoline alkaloids. His structure can be found in reference. The date of spectrum of berberine can be seen that the band at 1,396 cm-1 due to Ar-OCH3 deformation vibrations was greatly enhanced, indicating that the molecule was absorbed on silver gel strongly through lone-pair electron in Ar-OCH3. The ring stretching mode occurring around 1,548 cm-1 represents isoquinoline ring in the molecule. The band at 727 cm-1 due to CH (ring) deformation vibrations was also enhanced.

摘要

表面增强拉曼散射(SERS)与薄层色谱法(TLC)相结合已被用于研究微克级样品中分子的原位特征光谱。将SERS-TCL方法应用于中药有效成分研究的报道非常少。黄连是一种常用的临床中药。其主要有效成分包括黄连素等,具有广泛的抗菌作用,对改善心血管循环功能也有疗效。因此,黄连素的浓度对该药物的质量控制非常重要。在这项工作中,首先通过TLC分离黄连的乙醇提取物,然后在分离的斑点上滴加银胶后直接测量SERS。该方法可用于黄连素的指纹分析。将3微升总生物碱浓度为1.0毫克/毫升的黄连醇提取物置于硅胶GF254 TLC板上。样品用正丁醇-乙酸-水(7:2:1 V/V)展开剂进行分离。通过标准生物碱溶液确定样品中黄连素的位置。黄连素的Rf值为0.29。将银胶用作表面增强基底,置于分离的黄连素斑点上。用Nicolet FT-拉曼910光谱仪直接测量傅里叶变换表面增强拉曼光谱(FT-SERS)。黄连素属于异喹啉生物碱。其结构可在参考文献中找到。黄连素的光谱数据表明,由于Ar-OCH3变形振动在1396厘米-1处的谱带大大增强,表明该分子通过Ar-OCH3中的孤对电子强烈吸附在银胶上。在1548厘米-1左右出现的环伸缩模式代表分子中的异喹啉环。由于CH(环)变形振动在727厘米-1处的谱带也增强了。

需注意,原文中存在一些错误,比如“Coptis Chinensis France”表述有误,正确的是“Coptis chinensis Franch.” ;“Acitic acid”应是“Acetic acid” ;“His structure”应是“Its structure” ;“date of spectrum”应是“spectrum data” 。

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