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Study On Separation And Purfication Process Of Total Alkaloids From Sophoraflavescens AIT

Posted on:2016-12-30Degree:MasterType:Thesis
Country:ChinaCandidate:M Z XuFull Text:PDF
GTID:2284330470953116Subject:Pharmacy
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Objective:the application of Chinese medicine sophora was attaches great importance to the pharmaceutical industry,both in China and abroad in recent years,many scholars are actively using different methods from sophora in extraction and separation of its medicinal value of alkaloid,and traditional bitter ginseng total alkali extraction and separation technology, cycle is long,working procedure,the withdrawal rate is not high,the problem such as excessive use of organic solvent separation,the experiment of extraction and separation technology,on the basis of exploring the use of sophora medicinal materials contained alkaloids structural differences,using environmentally friendly solvents for the alkaloid extraction,separation by macroporous resin matrine,screening for organic solvents and pH liquid-liquid extraction, aqueous extraction using appropriate concentration of hydrogen peroxide solution to prevent the reduction of alkaloids,the separation of Sophora alkaloid,matrine、oxymatrine and oxysophocarpine of three kinds of new technology of alkaloids.Through the experiment a success.To achieve high yield, high purity,low energy consumption,low cost,the purpose of reducing environmental pollution.Methods.sophora alkaloid extraction condition optimizationn:in total alkaloid content of sophora and extraction rate as index,the diacolation extraction liquid ratio,solvent concentration,soaking time and extracting time on the single factor investigation;Sophora alkaloid optimization of separation and purification conditions:according to the bitter and salt or the free state of total alkaloid are soluble in water,the characteristics of the two to adjust pH value to make the alkaloid components in the form of precipitation to remove,achieve the goal of preliminary separated from impurities,further purification with macroporous adsorption resin sophora alkaloid,different types of macroporous adsorption resin for sophora alkaloid adsorption capacity and adsorption rate.resolution of three main factors,select the optimal macroporous resin,and the conditions on the column and elution conditions,the separation conditions were investigated.Results:optimizing the best diacolation extraction process is:the sophora meal with0.2%hydrochloric acid aqueous solution to fully immerse2hours later, using the diacolation method in material liquid ratio1:15,diacolation24hours in the extraction of sophora alkaloid composition,get diacolation liquid;Optimizing the sophora alkaloid separation,purification process is:diacolation liquid ammonia pH7,precipitation, filtration,adjustable pH9again, precipitation,filtration,the filtrate through macroporous adsorption resin column,column adsorption with5BV·h-1speed.Sophora alkaloid,acidic ethanol elution column with high volume fraction of acidic ethanol elution resin volume (about3times) as the column matrine, following a low volume fraction of acidic ethanol (about5times the volume of resin) elution oxide as the column bitter and alkali and alkali oxide sophora alkaloid.Will be bitter and alkaline cleaning liquid pressure off to concentrate syrups, matrine is tasted.It will be bitter and alkaline oxidation and oxidation alkaline wash sophora alkaloid to take off the liquid pressure relief to concentrate syrups, dissolve it in1times the amount of toluene and pH4aqueous solution of hydrochloric acid,hydrogen peroxide mix (toluene:acid water:hydrogen peroxide=1:2.5:1.2), extracting3times,bitter and alkali water phase to oxidation,organic phase oxidation of sophora alkaloid,decompression to concentrate syrups shape respectively, the use of acetone recrystallization,quick oxidation bitter sophora alkaloid and alkali and oxidation is tasted.Through the matrine、oxymatrine and oxysophocarpinethe physical and chemical indexes identification of sophora alkaloid, HPLC method,compared with medicinal materials contained in the corresponding alkaloids,10batches of matrine in small average yield of95.16%. Oxymatrine average yield of94.78%.Oxysophocarpinethe average yield of94.73%.Matrine purity97.98%.oxymatrine purity98.09%.oxysophocarpine purity98.07%.Certify that the above sophora alkaloid extraction and separation technology is a success. And the documents have not been reported.Conclusion:the use of sophora alkaloid into salt under acid condition,the characteristics of acid aqueous solution is helpful for the extraction of alkaloids,while flavonoids ingredients of sophora under the condition of acid insoluble in water, so the use of acid water extracted. Therefore,the use of polar macroporous resin.In from macroporous resin column separation of sophora alkaloid, the polarity of the use of matrine less bitter and alkali oxide and the characteristics of sophora alkaloid oxide with high volume fraction of acidic ethanol elution agent can be the first matrine elution down alone.For oxidation and alkali and alkali oxide sophora alkaloid similar polarity,on the premise of not use organic solvent,it’s hard to find a kind of environment-friendly eluent can be segmented elution two kinds of alkaloids,so the use of low volume fraction of acidic ethanol elution down to two kinds of alkaloids.Due to oxidation of sophora alkaloid may base on the molecular structure of double bond,is different from the oxidation of bitter and alkali,lipophilic after using it salt is different,with different polarity organic solvent and different pH value of water phase liquid liquid extraction.Finally successfully separate the two kinds of alkaloids,oxidation of sophora alkaloid reserves in organic phase toluene layer,oxidation and alkali transferred to the water phase.Extraction pH4acid to join a small amount of water in the process of bitter and alkaline hydrogen peroxide inhibits oxidation, oxidation reduction of sophora alkaloid.The experiment proved that according to the molecular structure of sophora alkaloid arising from the difference of physical and chemical properties of different.targeted to take corresponding extraction and separation method is feasible.The method has simple process,low cost and income each monomer alkaloids the advantages of high purity,suitable for industrial production.
Keywords/Search Tags:Sophora flavescens Ait., Oxymatrine, Oxysophocarpine, Matrine, Exttactionand separation and purification, Physical and chemical indicators
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