5种升麻中有机酸、色原酮和三萜皂苷的薄层色谱指纹图谱分析

Fingerprint analysis of organic acids,chromones and triterpenoid saponins in five Cimicifuga species by thin layer chromatography

目的:建立5种升麻的薄层色谱指纹图谱,并进行化学计量学分析。方法:样品经甲醇超声提取,点样于硅胶G预制板上,以三氯甲烷-甲醇-水(13∶7∶2)10℃以下放置的下层溶液为展开剂展开,于紫外光灯(365 nm)下检视并成像,再喷以茴香醛试液,于105℃加热至条斑清晰,置紫外光灯(365 nm)下检视并成像。图像经ChemPattern软件转换成数码轮廓图并生成共有模式后,进行相似度、二维聚类和主成分分析。使用升麻素、升麻苷、升麻亭、阿魏酸等6种对照品和QTofMS进行成分识别。结果:紫外光灯(365 nm)下,升麻色谱可见9个明显的淡蓝色条斑,显色后再置紫外光灯(365 nm)下,可见16个不同颜色的条斑,正品与非正品区别明显,3种正品的指纹图谱较为接近。结论:薄层色谱指纹图谱分析法适用于升麻的快速鉴别和质量控制。

Objective： To establish a method for fingerprint analysis and chemometric analysis of five Cimicifuga species by thin - layer chromatography （TLC）. Methods： The samples were extracted by ultrasonic with methanol, sample spotting for chromatography was performed on the silica gel 60 TLC plate, using the lower layer of a mixture of chloroform- methanol-water （13： 7： 2） stored below 10 ℃ as the developing solvent. The samples were exam- ined and their chromatograms were recorded in UV light at 365 nm, then in UV light at 365 nm after derivatization with anisaldehyde test solution （ heated at 105 ℃ ）. The images were converted to a digital profile with grayscale in- tensity and then the common pattern of TLC fingerprint was generated with ChemPattern software, and authentica- tion and quality assessment were conducted by similarity analysis, 2D cluster analysis and principal component a- nalysis. The compounds released by the bands were identified by six reference substances and QT of MS. Results： In the chromatogram of authentic Cimicifuga, nine light blue bands were visualized by UV light at 365 nm, sixteen characteristic bands with difference colors were visualized by UV light at 365 nm after derivatization with anisalde- hyde test solution. These bands could be easily distinguished from authentic Cimicifuga and the other species by comparison with the TLC chromatogram. The fingerprints of the three authentic Cimicifuga samples were generally i- dentical. Conclusion： The TLC fingerprint analysis method can be used for rapid identification and quality control of Cimicifuga.