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Study On Extraction, Purification And Quality Control Of Total Alkaloids In Summer

Posted on:2009-11-20Degree:MasterType:Thesis
Country:ChinaCandidate:J LiFull Text:PDF
GTID:2134360278471985Subject:Chinese materia medica
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Coyrdalis decumbentis (Thunb.)Pers. is a commonly used in Chinese herbs. The research has indicated that the alkaloids is its treatment of hemiplegia the main active ingredient. In recent years, the research is much concerned about the total Alkaloids. In order to study the advantages of resources, we mainly study the total alkaloids’extraction, separation、purification and quality control methods. A systematic study on the major findings are summarized as follows:In the conditions of extraction on the total Alkaloids, the total alkaloids and bicuculline’s extraction rate as an indicator, ethanol extraction methods and acid extraction methods were studied to determine the optimal extraction process:The Coyrdalis decumbentis were extracted for 3 times (24 hours/time) by using 0.5% hydrochloric acid, the amount of solvent were 4,3,3; The separated process studies the total alkaloids of Coyrdalis decumbentis, application macroporous resin technology from alkaloids of the different models of the three macroporous resin adsorption capacity static adsorption kinetics properties, dynamic performance and dynamic adsorption and desorption rate performance evaluation, select AB-8 macroporous resin adsorption, and AB-8 resin containing sample volume, eluting solvent study to determine the separation process Coyrdalis decumbentis:take extracts (relative density of 1.15, pH5), the AB-8 resin (high adsorption column diameter ratio 1:15, flow rate 3BV/h),5BV0.5mol/LNaOH elution solution and distilled water to wash neutral,3BV10% ethanol and 3BV90% ethanol eluting (3BV/h),90% ethanol eluate collection; Purification process of Coyrdalis decumbentis is 90% ethanol concentration ratio eluate, alkaline pH-value, drying methods and solvent addition salts inspection to determine purified process:90% ethanol concentration eluate to a relative density of 1:1.5 (concentrated liquid volume:volume of herbal medicine), dropping 10% sodium hydroxide solution (pH10), and leaving it overnight, filtering, washing Residue to neutral,65℃vacuum drying, drying times of health to join a drug dissolved in ethanol for 15min heating, filtration, the filtrate to a vacuum concentration crystallization,65℃vacuum drying.The quality control method use TLC,protopine、tetrahydropalmatine、bicuculline hydrochloride palmatine、berberin e and jatrorrhizine and other components were identified, and methods for carboxypeptidase A-cellulose sodium silica gel G adhesive plate, tertiary amine alkaloids chloroform-methanol-acetone-ammonia (20:1:2:3d)for the launch agent, quaternary ammonium alkaloids of ethyl acetate-chloroform-methanol-diethylamide(8:2:2:1) for the launch of an improved reagent bismuth potassium iodide for reagent, and the results showed the same color orange red dot, dot clear separation of good and the establishment of the TLC of Coyrdalis decumbentis; Acid dye assay used to the original protopine a total alkaloid content of the indicators, bromocresol green acid dyes for detection wavelength of 415nm, the content of quaternary ammonium, quaternary ammonium established in the determination of total alkaloids; The HPLC method was used to test for the Argentine protopine indicators, the use of C18 column, acetonitrile 0.1% trifluoroacetic acid (25:75) as the mobile phase, the detection wavelength was 290nm, the establishment of the central Plains coyrdalis decumbentis of a protopine determination; using HPLC, than bieueulline for detecting indicators, the use of C18 column, acetonitrile 0.1% trifluoroacetic acid (25:75) as the mobile phase, the detection wavelength was 225nm, established Coyrdalis decumbentis than bieueulline screening method. The bieueulline, the original A total alkaloids protopine and method for the determination of simple, with good precision and repeatability, and reliable determination applicable to Coyrdalis decumbentis quality control.
Keywords/Search Tags:Coyrdalis decumbentis, Total Alkaloids, Macroreticular resin, Determination of content
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