Study On The Preparation Method Of Rhubab And Gentian Extract To Traditional Chinese Medicine "Huanglong Siling Tang"

The formula of “Huang Longsiling” is a prescription on clinical treatment of hypertension and its complication.It consists of six herbs,including Rheum officinale,Radix gentianae,Polyporus umbellatus,Poria cocos,Rhizoma Alismatis and Rhizoma Atractylodis Macrocephalae.The main purpose of this paper is to study on the extraction and purification techonology of effective parts of the rhubarb and gentian,and to research the change of dissolubility of the effective components of the compatibility of both medicines.The main research overview as follows:1.The study of extraction and purification techonology on Rhubarb: A HPLC method was established to determine the five anthraquinone components content of aloe-emodin,rhein,emodin,chrysophanol,physcione in Radix et Rhizoma Rhei.Taking the extraction rate of contents of total anthraquinone as index,Cold-maceration extraction,warm immersion extraction,ultrasonic extraction,heating reflux extraction were adopted to extract Radix et Rhizoma Rhei respectively.4 kinds of extraction techonology were compared,The best extraction method is heat reflux extraction.Taking the extraction rate of contents of total anthraquinone as index,extraction technology was optimized by L9(34)orthogonal test by solvent concentration,extraction times and time,liquid-solid tatioas factors.The optimized extraction conditions were as follow: extracted 1h with 12 times 70% ethanol,andextracted 3 times.Taking the extraction rate of contents of total anthraquinone as index,and using macroporous adsorption resin column chromatography to purify the crude extract of rhubarb.Ivestigate the adsorption and desorption ability of the the nine kinds of macroporous adsorption resin,and the best resin model to purify the rhubarb effective parts was D101.And using the single factor experiment with L9(34)orthogonal experiment method to optimize the craft parameters of the macroporousresin.The optimized purification technology was as following: the ratio of colum diameter is 3:1,the concentration of sample solution 0.1g/m L with adsorption velocity 4BV/h,sample capacity 54 m L,then eluted with 7BV 60% ethanol at the speed of 2BV/h,collected eluate.Under these conditions,yield of total anthraquinone was 47.89%.2.The study of extraction and purification techonology on gentiopicroside:A HPLC method was established to determine the content of gentiopicroside.Taking the extraction rate of gentiopicroside as index,Cold-maceration extraction,warm immersion extraction,ultrasonic extraction,heating refluxextraction were adopted to extract gentiopicroside respectively.4 kinds of extraction techonology were compared,The best extraction method is heat reflux extraction.Taking the extraction rate of gentiopicroside as index,extraction technology was optimized by L9(34)orthogonal test by solvent concentration,extraction times and time,liquid-solid tatioas factors.The optimized extraction conditions were as follow: extracted 1h with 10 times 70% ethanol,andextracted 3 times.Taking the extraction rate of contents of total anthraquinone as index,and using macroporous adsorption resin column chromatography to purify the crude extract of radixgentianae.Ivestigate the adsorption and desorption ability of the nine kinds of macroporous adsorption resin,and the best resin model to purify the radixgentianae effective parts was SP700.And using the single factor experiment with L9(34)orthogonal experiment method to optimize the craft parameters of the macroporousresin.The optimized purification technology was as following: the ratio of colum diameter is 9:1,the concentration of sample solution 0.1g/m L with adsorption velocity 4BV/h,sample capacity 135 m L,then eluted with 6BV 30% ethanol at the speed of 1BV/h,collected eluate.Under these conditions,yield of gentiopicroside was 49.84%.3.Influence of compatibility of Rhubarb with radixgentianae on the extraction and dissolution of effective parts of both:Adopting the system of HPLC-DAD,to determine the aloe-emodin,rhein,emodin,chrysophanol,physcione in Radix et Rhizoma Rhei and the gentiopicroside in radixgentianae at the same time,with Agilent C18 reversed-phase chromatography(4.6mm×250mm,5μm),methanol-0.02% phosphoric acid solution as mobile phase with a gradient elution,detector wavelength: 254 nm and 270 nm.Under the optimum extraction conditions of Rhubarb and Gentianae respectively,the rhubarb-gentian extracted by different proportion,and the dissolution compositions of five anthraquinone components and gentiopicroside were detected by HPLC,and data were analyze.The results showed that the extraction of Rhubarb-Gentian have a certain influence on the dissolubility of effective components.the dissolution quantity of effective parts varies with the change of the compatibility proportion of Rhubarb-Gentian,and there were significant differences.