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The Chemical Research Of Alkalescenr Alkaloids In Crinum

Posted on:2015-04-15Degree:MasterType:Thesis
Country:ChinaCandidate:S T WangFull Text:PDF
GTID:2404330491960195Subject:Pharmacy
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Cancer is one of the most serious diseases theeatening human health,while,the traditional chemotherapy has not only have toxicity,poor selectivity but also has the multiple drug resistance.However,the natural plant extract can inhibit tumor cells of high-efficiency compound has important significance for medical field.The alkaloid of Crinum is a kind of isoquinoline alkaloid,has significant anti-tumor activity,it has attracted the wide attention.Plants of Amaryllidaceae are often used to treat phlegm,detoxification,edema,sore throat a carbuncle evil nuclear and diuretic.In recent years,research have found that plants of Amaryllidaceae have effect on central nervous system,the role of a variety of bacteria resistant,can effect the cardiovascular system and have anti-viral effect,have significantly effect of inhibited tumor cells.Crinum of Amaryllidaceae is widely used as the analgesic and anti-inflammatory treatment of other diseases.Currently,less of study about Crinum,it have essential to Crinum comprehensive analysis of alkaloids,get alkalescent alkaoids feom Crinum.The study of alkalescent alkaoids of Crinum chemical provide strong experimental evidence for the clinical use of Crinum alkaloids provide effective reference data for clinical,scientific theoretical basis for the development of efficient and low toxicity of TCM drugs.In this paper,the classical chemical methods are used for extracted the seed of Crinum alkaloid and investigated Crinum total alkaloid is extraction by orthogonal method.Because of the different between the basic alkaloids,alkaloids with acidic water to dissolve the salt,Because of the different between the basic alkaloids,alkaloids with an acidic aqueous solution so it can dissolved the salts,adding alkali pH values in ascending order.Identified by thin layer chromatography on alkalescenr alkaloids in Crinum unfold separated stationary phase silica gel with ethyl acetate-methanol,the use of potassium iodide,bismuth identified,was two spots,to provide a reference for the column chromatography filters.By column chromatography on alkalescent alkaline of Crinum separation and purification,the stationary phase is silica gel,move to methanol-ethyl acetate gradient.Two samples analyzed by HPLC.Therefore,the use of liquid chromatography-mass spectrometry for weakly basic alkaloids Crinum two samples for qualitative analysis to speculate further analyze for its molecular weight.Determined by the method of appeal to the optimum extraction of alkaloids from Crinum total of 85%ethanol concentration,extraction temperature is 65?,extraction 3h.After the dissolution of the total alkaloids hydrochloric acid to adjust pH=4,ethyl acetate three times to no alkaloids color reaction,have Crinum alkalescent alkaloids.Screening by TLC on silica stationary phase,eluent,ethyl acetate:methanol=3:14.When expand to Rf 0.333 and 0.712.In the experiment,column chromatography,ethyl acetate:methanol=100:1 to ethyl acetate:methanol=10:6 as components of the sample collection,the use of a thin layer of unfold Rf=0.712,combined and evaporated,and the resulting sample as the 1st sample.Ethyl acetate:methanol=10:9 to ethyl acetate:methanol=1:1 collected fractions by thin layer unfold Rf=0.333.Combined and evaporated,and the result sample is the sample number 2.The resulting two-component samples were analyzed by HPLC,the moved phase through the filter,the final choice of methanol-water gradient elution,wherein the proportion of methanol is 10%-100%water ratio of 90%-0 elution time of 1 h.The final two-component samples were analyzed by HPLC,the moved phase through the filter,the final choice of methanol-water gradient elution,wherein the proportion of methanol is 10%-100%water ratio of 90%-0%elution time of 1h.The use of LC-MS for two samples for further analysis,the use of proceeds from the molecular weight of the final Crinum presumably weak alkaline alkaloids Latifoliumprine,Latifoliumdne,Lyeorenan-7-one,LatifoliuminB,Uridine,Ungeremine,Lycorenium A,1-methyl-lH-pyrimidine-2,4-dione,NareiPrimin,Arolyeorieidin,eight kinds of alkaloids.
Keywords/Search Tags:Crinum, alkaloids, Column chromatography, LC-MS
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