应用TLC-CMS-IR技术检测北芪菇中黄芪甲苷

Astragalus Glycoside in Astragali Mushroom Detected by TLC-CMS-IR

以乙醇水溶液为提取剂,从北芪菇中提取黄芪甲苷,薄层层析(TLC)分离和制备黄芪甲苷;通过对比质荷比(m/z)和官能团等对黄芪甲苷进行表征与分析。结果表明,乙醇-水=7∶3(V/V)作为提取剂,微波超声波处理后,多级萃取后得到正丁醇相;氯仿∶甲醇∶乙酸乙酯∶水=13∶7∶2∶2(V/V)展开后,经显色获得的色谱斑点与黄芪甲苷标准品斑点位置比对一致,Rf值为0.31;黄芪甲苷样品和标准品质谱波谱图和红外波谱图确定提取物为黄芪甲苷。样品中黄芪甲苷的熔点是295℃;旋光度是+56.4;比旋光度是+24.4。结果表明,TLC-MS-IR联用是一种具有独特优势的色谱波谱技术,能实现从微克量级的分离分析到克量级的分离制备,可用于天然产物粗提物的去除杂质和单个产物的精制,适用于从北芪菇中进行物质的制备分离。

The crude extracts of astragalus glycoside from Astragalus japonicum were obtained by multistage extraction.Thin layer analysis and purification were used to obtain Astragalus actinosine,and qualitative analysis of Astragalus actinosine in Beiqi mushroom was conducted by mass spectrometry and infrared analysis.Finally,the melting point,rotation degree,and specific rotation photometry of Astragalus actinosine were determined.Display∶ethanol-water(7∶3)was used as extraction agent.After microwave ultrasonic treatment,the upper phase of n-butanol was obtained after multistage extraction.With chloroform∶methanol∶ethyl acetate∶water=13∶7∶2∶2 as expansion agent,need spots,obtained with thin-layer chromatography with standard astragalus armour glycosides spots than confirmation for astragalus armour glycosides.The extraction of astragaloside was determined by analysis of samples and standard mass spectrometry and ir spectrometry.Astragalus armour glycosides in the sample melting point was 295℃;The rotatory power was+56.4;The specific rotation was+24.4.TLC-MS-IR spectrometry was a kind of unique advantage of chromatographic spectrum technology,could realized from micrograms of separation of level analysis to g level of preparation,separation can be used for crude extractings from natural products refined to remove impurities and individual products,suitable for material preparation of separation from astragali mushroom.