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Separation And Analysis Of Spreading Hedyotis Herb And Other Chinese Medicine Effective Component

Posted on:2016-10-27Degree:MasterType:Thesis
Country:ChinaCandidate:X Y DingFull Text:PDF
GTID:2284330479477554Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
Although China has the world’s most abundant resources of Chinese herbal medicine,due to the complex chemical components, the lack of quantitative standard product quality and the unstable product quality, and most of the single and compound preparations of effective material basis is unclear, thus establishing a quick and effective purification method of chemical composition of traditional Chinese medicine has a realistic significance.In this paper, through the study of Chinese herbal medicine chemical purification methods, To establish a new method of extraction and separation of active ingredients from Hedyotis diffusa Willd, Hypericum performatum L. and Milk thistlea. In experiments using high performance liquid chromatography(HPLC) as a means of detection, to analysis various material crude extract and purity of monomer, and optimize the conditions for testing, Using the type of preparation of high performance liquid chromatography(PHPLC) and column chromatography to separate and purify the target compounds,Finally using ultraviolet(UV) and nuclear magnetic resonance spectroscopy(NMR) to identify the chemical structure of the target compounds.3.Isolation and purification methods of active ingredients from Hedyotis diffusa WilldChemical composition of spreading hedyotis herb extraction process was studied,established the optimal extraction process: extraction solvent was 95% ethanol, extraction method was heated to reflux for 3 hours by 4 times. With petroleum ether, ethyl acetate,n-butyl alcohol extracting concentrated extract in turn. Extract of the three parts carries on the preliminary separation by silica gel column, Then useing PHPLC for further purification. It is concluded that two kinds of sterol compounds, Anthraquinone compounds and of flavonoids each have five kinds. Finally identified the structure by HPLC, UV, NMR.4.Isolation and purification methods of active ingredients from Hypericum performatum L.A new method for separation and purification of the naphthodianthrones fromHypericum performatum L.was established by polyamide column and ODS column. First,the Hypericum perforatum L.was extracted by ultrasonic extraction in ethyl acetate,Concentrated extract was purified by polyamide column, and eluted with 95% ethanol and acetone in turn, collecting the acetone eluent. Then the final separation and purification of the acetone elution composition by ODS column. Their structures were identified by UV and NMR, and eventually getting hypericin and emodin anthrone, the purity of 95.8% and99.8% respectively.4.Isolation and purification methods of silymarin from Milk thistleaFirstly, Isolation and purification of silymarin get five compounds from Milk thistle by PHPLC. The optimized PHPLC chromatographic conditions for: Chromatographic column was ODS-A(400mm×40mm,I.D.10μm),Mobile phase was methanol and water(50:50 v/v),Sample quantity was 1m L, The velocity was 25 m L/min, Detection wavelength was 288 nm,The elapsed time was 60 min. Separation of Milk thistle extract directly use PHPLC technology, running time was too long, solvent consumption was big, and efficiency was low. So a second purification method is established, multi-stage extraction method. The silymarin composition is divided into two parts by this method, separation and purification of the two parts respectively use PHPLC technology again. Finally the extraction of water phase get three kinds of compounds: They were silychristin, silydianin and silybin A.Organic phase part get two kinds of compounds: They were silybin B and isosilybin A. The structure identified by UV and NMR, All the purity were greater than 95%.
Keywords/Search Tags:Preparation of high performance liquid chromatography(HPLC), Column chromatography, Isolation and purification, Hedyotis diffusa Willd, Hypericum performatum L., Milk thistlea
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