Study On Industrial Extraction And Separation Technology Of Baicalin

In this thesis,the author has carefully studied the production technology and testing methods of Baicalin in Scutellaria baicalensis in depth. Finally, an effective experimental data was made and the experimental result was concluded and analysed theoretically. The clear production route, full and accurate experimental data will provides reference for the industrial production.1. Thin layer chromatography, Spectrophotometry and High Performance LiquidChromatography are methods which mainly be used to analyse and test Baicalin.The thin layer chromatography:TLC plate is silica gel G plate; a mixture of acetum,aldol,water (acetum:aldol:water=6:1.5:2.5)works as developing solvent; the extracts were colorated with a2%solution of AlCl3and ethanol spray. Because the thin layer chromatography method doesn't need expensive instrument,it is simple and convenient, it usually be used as the method to examine Baicalinon on the product line.The High Performance Liquid Chromatography:Chro-matographic conditions were: Using C18column with acetum,aldol and water solution (5:5:1) as the mobile phase,dvelocity at1.0mL/min,etection wavelength at280nm and injection volume was20ul., room temperature.The High Performance Liquid Chromatography which has high resolution and detection speed as well as accuracy is the mostly used method for Baicalin testing.2. The analysis of Baicalin content in Scutellaria baicalensis from different original producing areas, picking seasons, parts shows that Baicalin contents are various. Therefor,the plantation area,original producing area and pcking seasons should be considered. Baicalins are distributed in root,velamen,fibrous root and Fibrous root bark.so, all of this parts ahould be choosed as production materials.3.Mono-factor experiments and orthogonal experiments showed that the best production technology was as follows:using the hot reflux methods to extract Baicalin from Scutellaria baicalensis podwer, in75%alcohol Solvent, the ratio of raw material and solvent is1:15, extract two times under reflux,90min at a time.4.The result of the clarilification experiment showed that using1%aluminium potassium sulfate to treat extract will help us to get the suitable liquid on the column.5.The static and dynamic Macroporous Absorbing Resin experiment showed that:the AB-8Macroporous Resins was the best adsorbent to purify and enrich Baicalin. The Experimental parameters were as follows:the concentration in extracted solution was about10.0mg/ml, the extracted solution was5BV,sample flow velocity of3-5ml/min,eluted with50%6BV acohol solution, eluting velocity of5-8ml/min.Under such conditions, there would be the production whose purity was over60%and after further purified,the purity was above85%.6.Determined the enlarging experiment technology on extraction and separation experimental result of Baicalin according on the Mono-factor experiments,Orthogonal experiments and the Static and Dynamic Macroporous Absorbing Resin experiment:To weight the raw Scutellaria baicalensis powder which was sifted through a0.20mm sieve, to ensure3times75%ethanol,circumfluence distilling3times and1.5hours every time. The production of the third time was the extraction solvent which would be used for the next time. After rough fractionation, then mixed with1%aluminium potassium sulfate of the raw material weight, stirred well, weakening by the addition of distilled water,filtered and removed the undissolved substance by frame, then got the pure column liquid.keeping standing0.5h,and then filtered again,got the AB-8macroporous resin column,to elute with6BV50%ethanol, colleted the eluted liquid, concentrated,dried and crushed,then obtained rough product; or colleted the eluted liquid,concentrated under reduced pressure, obtained the deposit,crushed and got the rough product, recrystallizated and obtained the superior Baicalin.7. The result in pilot plant scale experiments on extracting Baicalin from Scutellaria baicalensis indicated that the ratio of rough product Baicalin is8.97%, the Baicalin content is50.35%,the rough and Competitive product is5.48%,, the Baicalin content is85.79%; the Competitive product of Baicalin is2.17%and the Baicalin content is95.09%.