CN104983836A - Method for extracting active components from compound blood lipid ning bulk drugs - Google Patents
Method for extracting active components from compound blood lipid ning bulk drugs Download PDFInfo
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Abstract
The invention discloses a method for extracting active components from compound blood lipid ning bulk drugs. The method comprises the following steps: the compound blood lipid ning bulk drugs are added into a beta-cyclodextrin solution to be soaked for 1 hour, reflux extraction is carried out on the bulk drugs and the beta-cyclodextrin solution 1 time to 3 times, the reflux extraction time each time ranges from 1 hour to 2 hours, and the using amount of the beta-cyclodextrin solution accounts for 5% to 15% of the total weight of the compound blood lipid ning bulk drugs; and the material-solution ratio of the compound blood lipid ning bulk drugs to the beta-cyclodextrin solution is 1:25-1:15. Compound blood lipid ning is taken as a model drug, the lipid-lowering active components in the compound blood lipid ning are taken as an index, on the basis of the molecule selecting clathration of the cyclodextrin, the whole extraction research on Chinese herbal compound multi-active components with the beta-CD as the carrier is carried out, and the proper extraction method is obtained to effectively maintain the pharmacological activity of the traditional Chinese medicine compound blood lipid ning activity.
Description
Technical field
The present invention relates to a kind of method extracting active component from the crude drug of compound recipe XUEZHINING.
Background technology
Cyclodextrin (Cyclodextrin is called for short CD) is the product that starch Bacillus alcalophilus is formed after cultivating the cyclodextrin glucanotransf translocase effect obtained.Be the cyclic oligomer sugar compounds connected with Isosorbide-5-Nitrae-glycosidic bond by 6-12 D-Glucose molecule, be water solublity, irreducibility white crystals sprills, common are α, and beta, gamma three type is made up of 6,7,8 glucose molecules respectively.Especially the most conventional with β-CD.CD structure hollow tube-shape circlewise, ring cylinder outside is hydrophilic surface, and inner non-polar group forms the hydrophobic cavity that has certain size.
Due to the special construction that cyclodextrin is circular hollow cylinder type, therefore present a series of special nature, can with Cucumber molecule forming bag mixture.The outer field macromolecular substances of clathrate is called " host molecule ", is wrapped and material in host molecule is called " enclosed molecule ".Clathrate is make to be formed in guest molecule all or part of embedding cyclodextrin molecular cave by hydrophobic interaction, hydrogen bond and Van der Waals force between Subjective and Objective molecule.Make, by the physicochemical property of enclose medicine and biological property, significantly change is occurred, be thus widely applied in fields such as Chemical Decomposition and analysis, drug controlled release, organic synthesis and catalysis, food processing and environmental conservation.
Chinese medicine compound XUEZHINING is recorded in the version Pharmacopoeia of the People's Republic of China one in 2010, is made up of, has blood-activating and qi-promoting, effect of blood stasis dispelling blood fat reducing Semen Cassiae, Radix Polygoni Multiflori Preparata, Folium Nelumbinis, Fructus Crataegi four taste Chinese medicine, is applicable to the stagnant caused hyperlipemia of the blood vessels stasis of blood.
Chinese medicine has very long developing history, has the features such as of a great variety, of many uses, contained chemical composition is various, pharmacological action is complicated, due to the clinical efficacy that it is good, receives the welcome of the people of other countries.Along with science and technology and the progress of research means and raising, also more and more deep to the research of Chinese medicine, the particularly Study on extraction of Chinese medicine.Because Mechanism of TCM is complicated, according to the difference of its property of medicine and active component, suitable extracting method is selected effectively to keep the pharmacologically active of active ingredient of Chinese herbs to seem particularly important.
Summary of the invention
An object of the present invention is to solve at least the problems referred to above and/or defect, and the advantage will illustrated at least is below provided.
A further object of the invention is to provide a kind of method extracting active component in crude drug of compound recipe XUEZHINING, the present invention with compound recipe XUEZHINING for model drug, with Lipid-lowering activities composition wherein for index, based on the Molecular Selection clathration of cyclodextrin, carry out and for carrier, research is extracted to the entirety of Chinese medicine compound various active composition with β-CD, obtain the pharmacologically active that suitable extracting method keeps Chinese medicine compound XUEZHINING activity effectively.
A further object of the invention is to provide the purposes of beta-schardinger dextrin-in the crude drug extracting compound recipe XUEZHINING in active component method.
For this reason, technical scheme provided by the invention is:
A kind of method extracting active component from the crude drug of compound recipe XUEZHINING, comprise the steps: the crude drug of compound recipe XUEZHINING to join in beta-schardinger dextrin-solution to soak 1h, afterwards the mixed-liquor return of described crude drug and beta-schardinger dextrin-solution is extracted 1 ~ 3 time, each return time is 1 ~ 2h, wherein, the consumption of beta-schardinger dextrin-accounts for 5% ~ 15% of the crude drug gross weight of described compound recipe XUEZHINING, and the crude drug of described compound recipe XUEZHINING and the solid-liquid ratio of described beta-schardinger dextrin-solution are 1:25 ~ 1:15.
Preferably, described extracts in the method for active component from the crude drug of compound recipe XUEZHINING, and the consumption of beta-schardinger dextrin-accounts for 5% of the crude drug gross weight of described compound recipe XUEZHINING.
Preferably, described extracts in the method for active component from the crude drug of compound recipe XUEZHINING, and the crude drug of described compound recipe XUEZHINING and the solid-liquid ratio of described beta-schardinger dextrin-solution are 1:25.
Preferably, described extracts in the method for active component from the crude drug of compound recipe XUEZHINING, is joined in beta-schardinger dextrin-solution by the crude drug of compound recipe XUEZHINING and soaks 1h, afterwards heating and refluxing extraction 3 times.
Preferably, described extracts in the method for active component from the crude drug of compound recipe XUEZHINING, and in described reflux, each return time is 2h.
Preferably, described extracts in the method for active component from the crude drug of compound recipe XUEZHINING, the crude drug of described compound recipe XUEZHINING comprises Semen Cassiae, Radix Polygoni Multiflori Preparata, Folium Nelumbinis and Fructus Crataegi, and the part by weight of described Semen Cassiae, Radix Polygoni Multiflori Preparata, Folium Nelumbinis and Fructus Crataegi is 3:2:1.5:1.
Even more preferably, described extracts in the method for active component from the crude drug of compound recipe XUEZHINING, and also containing mass body volume concentrations in described beta-schardinger dextrin-solution is the EDTA of 0.08mg/mL, and the pH of described beta-schardinger dextrin-solution is 2.5 ~ 3.0.
Preferably, described extracts in the method for active component from the crude drug of compound recipe XUEZHINING, and first being pulverized by the crude drug of compound recipe XUEZHINING is 100 object granules, joins in beta-schardinger dextrin-solution afterwards again and soaks.
Even more preferably, described extracts in the method for active component from the crude drug of compound recipe XUEZHINING, the 1st time of reflux, extract, certain time through four-stage and under each stage successively, first first stage refluxes to the liquid of 70% of the described mixeding liquid volume of described crude drug and beta-schardinger dextrin-solution, second, third and fourth stage add 1/3 of residual mixed liquor volume more respectively and reflux afterwards, wherein, the described first stage continues 40min, described second and the phase III respectively continue 20min, described fourth stage continues 40min.
Preferably, described extracts in the method for active component from the crude drug of compound recipe XUEZHINING, and described active component comprises rubrofusarin-6-O-β-D-O-gentibioside, stilbene glucoside, emodin, nuciferine and Quercetin.
The present invention at least comprises following beneficial effect: beta-schardinger dextrin-have nontoxic, to the advantage such as thermally-stabilised and cheap and easy to get, the present invention adopts the active component in beta-schardinger dextrin-complementary extraction Chinese medicine compound XUEZHINING, and the extraction rate of transform of index components all has significance to improve.Also containing mass body volume concentrations in beta-schardinger dextrin-solution of the present invention is the EDTA of 0.08mg/mL, and its pH is 2.5 ~ 3.0.Under this pH environmental condition, EDTA can promote that beta-schardinger dextrin-plays effect larger, strengthens the active force of beta-cyclodextrin inclusion compound active component, makes clathration stronger, to improve the extraction rate of transform to active component further.In order to beta-schardinger dextrin-contacts more fully with crude drug, first the crude drug of compound recipe XUEZHINING is pulverized by the present invention is 100 object granules, joins in beta-schardinger dextrin-solution afterwards again and soaks.The 1st time of reflux, extract, successively through four-stage and under each stage certain time carry out, improve efficiency and the extraction effect of backflow.Compared with traditional water extraction, β-CD has significant complementary extraction effect to index components, the extraction rate of transform of active component can be improved significantly, enhance the controllability of compound recipe XUEZHINING extraction process, make it extract efficient, energy-conservation, controlled, the application in compound recipe XUEZHINING extraction process has further researching value.
Part is embodied by explanation below by other advantage of the present invention, target and feature, part also will by research and practice of the present invention by those skilled in the art is understood.
Accompanying drawing explanation
figure 1Aillustrate the chromatograph of a sample
figure, wherein,
figure 1Ain 1 represent nuciferine, 2 generations
table twostyrene glycosides, 3 represents rubrofusarin-6-O-β-D-O-gentibioside, 4 and represents Quercetin, 5 and represent emodin.
figure 1Billustrate the chromatograph of reference substance
figure,
figure 1Bin 1 represent nuciferine, 2 generations
table twostyrene glycosides, 3 represents rubrofusarin-6-O-β-D-O-gentibioside, 4 and represents Quercetin, 5 and represent emodin.
fig. 2 Afor different feed liquid is than the extraction rate of transform of lower rubrofusarin O-gentibioside
figure.
fig. 2 Bfor different feed liquid is than the extraction rate of transform of lower stilbene glucoside
figure.
fig. 2 Cfor different feed liquid is than the extraction rate of transform of lower emodin
figure.
fig. 2 Dfor different feed liquid is than the extraction rate of transform of lower nuciferine
figure.
fig. 2 Efor different feed liquid is than the extraction rate of transform of lower Quercetin
figure.
fig. 3for the comparison of the extraction rate of transform of five kinds of compositions in the Different Extraction Method in the present invention
figure, wherein,
fig. 3in 1 identification post body display hot dipping extract the extraction rate of transform of five kinds of compositions in (80 DEG C) method, the extraction rate of transform of five kinds of compositions in 2 identification post body display ultrasonic extracting methods, the extraction rate of transform of five kinds of compositions in 3 identification post body display reflux extraction method.
fig. 4 Afor the extraction rate of transform of rubrofusarin O-gentibioside under different extraction time
figure.
fig. 4 Bfor the extraction rate of transform of stilbene glucoside under different extraction time
figure.
fig. 4 Cfor the extraction rate of transform of emodin under different extraction time
figure.
fig. 4 Dfor the extraction rate of transform of nuciferine under different extraction time
figure.
fig. 4 Efor the extraction rate of transform of Quercetin under different extraction time
figure.
fig. 5 Afor the extraction rate of transform of rubrofusarin O-gentibioside under different extraction time
figure.
fig. 5 Bfor the extraction rate of transform of stilbene glucoside under different extraction time
figure.
fig. 5 Cfor the extraction rate of transform of emodin under different extraction time
figure.
fig. 5 Dfor the extraction rate of transform of nuciferine under different extraction time
figure.
fig. 5 Efor the extraction rate of transform of Quercetin under different extraction time
figure.
fig. 6 Afor the extraction rate of transform of rubrofusarin O-gentibioside under different beta-CD consumption
figure.
fig. 6 Bfor the extraction rate of transform of stilbene glucoside under different beta-CD consumption
figure.
fig. 6 Cfor the extraction rate of transform of emodin under different beta-CD consumption
figure.
fig. 6 Dfor the extraction rate of transform of nuciferine under different beta-CD consumption
figure.
fig. 6 Efor the extraction rate of transform of Quercetin under different beta-CD consumption
figure.
fig. 7for the comparison of the extraction rate of transform of five kinds of compositions in the extraction with aqueous solution in the present invention and β-CD extracting method
figure,
in figure* represents there is significant difference, P<0.01 compared with water extraction,
fig. 7middle A shows the extraction rate of transform of five kinds of compositions in aqueous extraction process,
fig. 7middle B shows the extraction rate of transform of five kinds of compositions in β-CD extracting method.
Detailed description of the invention
Below in conjunction with
accompanying drawingthe present invention is described in further detail, can implement according to this with reference to description word to make those skilled in the art.
The invention provides a kind of method extracting active component from the crude drug of compound recipe XUEZHINING, comprise the steps: the crude drug of compound recipe XUEZHINING to join in beta-schardinger dextrin-solution to soak 1h, afterwards the mixed-liquor return of described crude drug and beta-schardinger dextrin-solution is extracted 1 ~ 3 time, each return time is 1 ~ 2h, wherein, the consumption of beta-schardinger dextrin-accounts for 5% ~ 15% of the crude drug gross weight of described compound recipe XUEZHINING, and the crude drug of described compound recipe XUEZHINING and the solid-liquid ratio of described beta-schardinger dextrin-solution are 1:25 ~ 1:15.
The present invention adopts the active component in beta-schardinger dextrin-complementary extraction Chinese medicine compound XUEZHINING, the extraction rate of transform of active component can be improved significantly, enhance the controllability of compound recipe XUEZHINING extraction process, make it extract efficient, energy-conservation, controlled, the application in compound recipe XUEZHINING extraction process has further researching value
As preferably, the consumption of beta-schardinger dextrin-accounts for 5% of the crude drug gross weight of described compound recipe XUEZHINING.
As preferably, the crude drug of described compound recipe XUEZHINING and the solid-liquid ratio of described beta-schardinger dextrin-solution are 1:25.
As preferably, the crude drug of compound recipe XUEZHINING is joined in beta-schardinger dextrin-solution and soaks 1h, afterwards heating and refluxing extraction 3 times.
As preferably, in described reflux, each return time is 2h.
As preferably, the crude drug of described compound recipe XUEZHINING comprises Semen Cassiae, Radix Polygoni Multiflori Preparata, Folium Nelumbinis and Fructus Crataegi, and the part by weight of described Semen Cassiae, Radix Polygoni Multiflori Preparata, Folium Nelumbinis and Fructus Crataegi is 3:2:1.5:1.
As preferably, be also the EDTA of 0.08mg/mL containing mass body volume concentrations in described beta-schardinger dextrin-solution, the pH of described beta-schardinger dextrin-solution is 2.5 ~ 3.0.Under this pH environmental condition, EDTA can promote that beta-schardinger dextrin-plays effect larger, strengthens the active force of beta-cyclodextrin inclusion compound active component, makes clathration stronger, to improve the extraction rate of transform to active component further.
As preferably, in order to beta-schardinger dextrin-contacts more fully with crude drug, first being pulverized by the crude drug of compound recipe XUEZHINING is 100 object granules, joins in beta-schardinger dextrin-solution afterwards again and soaks.
As preferably, for improving efficiency and the extraction effect of backflow, the 1st time of reflux, extract, certain time through four-stage and under each stage successively, first first stage refluxes to the liquid of 70% of the described mixeding liquid volume of described crude drug and beta-schardinger dextrin-solution, and second, third and fourth stage add 1/3 of residual mixed liquor volume more respectively and reflux afterwards.In reflux, extract, the described first stage continues 40min, described second and the phase III respectively continue 20min, described fourth stage continues 40min.
As preferably, described active component comprises rubrofusarin-6-O-β-D-O-gentibioside, stilbene glucoside, emodin, nuciferine and Quercetin.
Compound recipe XUEZHINING is made up of four taste Chinese medicines such as Semen Cassiae (30g), Radix Polygoni Multiflori Preparata (20g), Folium Nelumbinis (15g), Fructus Crataegis (10g), there is blood-activating and qi-promoting, effect of blood stasis dispelling blood fat reducing, is applicable to the stagnant caused hyperlipemia of the blood vessels stasis of blood.Modern pharmacology research shows to have multiple drug activity composition in XUEZHINING.The present invention is derived from from the compound recipe XUEZHINING identified in 17 compositions Semen Cassiae, Radix Polygoni Multiflori Preparata, Folium Nelumbinis, have chosen the evaluation index of drug activity composition as the complementary Study on extraction of β-CD of 5 kinds of structure types: rubrofusarin-6-O-β-D-O-gentibioside, stilbene glucoside, emodin, nuciferine and Quercetin.First by carrying out single factor exploration to solid-liquid ratio, extracting method, β-CD consumption etc., further design orthogonal test is studied β-CD complementary extraction compound recipe XUEZHINING technique, sums up β-CD to the selective extraction rule of five kinds of compositions and each factor to the impact of its selective extraction.
Embodiment 1
1. material
1.1 medicine
Nuciferine (111566-200703), Quercetin (100081-200907), emodin (110756-200110), chrysophanol (110796-201017) are purchased from National Institute for Food and Drugs Control; Rubrofusarin-6-O-β-D-O-gentibioside (purity >=98%) opens up marine growth Science and Technology Ltd. purchased from Nanjing; Stilbene glucoside (purity >=98%) is self-control.
Semen Cassiae (place of production: Vietnam), Radix Polygoni Multiflori Preparata (place of production: Sichuan), Folium Nelumbinis (place of production: Shandong), Fructus Crataegi (place of production: Chengde).
1.2 reagent
1.3 instrument
2. method and result
2.1 chromatographic condition
Chromatographic column: Acquity UPLC BEH shield RP18 (2.1 × 100mm, 1.7 μm); Mobile phase: methanol (A)-0.1% aqueous formic acid (B), gradient elution program is shown in
following table 1; Flow velocity: 0.2ml/min; Column temperature: 45 DEG C; Detection method adopts wavelength to switch method, specifically sees
table 2; Analysis time: 40min; Sample size 3 μ L.Chromatograph
figuresee
figure 1Awith
figure 1B,
figure 1Aillustrate the chromatograph of sample
figure,
figure 1Billustrate the chromatograph of reference substance
figure, wherein,
figure 1Awith
figure 1Bin 1 represent nuciferine, 2 generations
table twostyrene glycosides, 3 represents rubrofusarin-6-O-β-D-O-gentibioside, 4 and represents Quercetin, 5 and represent emodin.Wherein the preparation of reference substance storing solution is as described in 2.2.1, and sample is a sample of random selecting.From
figure 1Awith
figure 1Bin, can find out that chromatographic condition is good, be suitable for measuring this five kinds of compositions.
table 1gradient elution
table
table 2wavelength switches
table
2.2 methodological study
2.2.1 linear relationship and detectability
Take rubrofusarin O-gentibioside, stilbene glucoside, emodin, nuciferine and Quercetin reference substance respectively appropriate, be placed in 10mL volumetric flask, with methanol constant volume, obtain concentration and be followed successively by 536 μ g/mL, 1050 μ g//mL, 492 μ g/mL, reference substance storing solution five kinds of composition reference substances of 168 μ g/mL, 503 μ g/mL are appropriate, draw reference substance appearance liquid respectively and are mixed into reference substance solution in right amount, stepwise dilution becomes the reference substance solution of a series of variable concentrations, and sample introduction measures peak area.With reference substance concentration (c), for vertical coordinate, linear regression analysis is carried out to peak area (A), obtain the equation of linear regression of each composition, the range of linearity and correlation coefficient, the results are shown in
table 3.
table 3measure components regression equation, correlation coefficient, the range of linearity
2.2.2 precision
Prepare each composition and working sample responds close mixed mark solution, measure peak area by chromatographic condition sample introduction 6 pin under " 2.1 " item, calculate precision.
as table 4shown in, result shows that the RSD value of 5 compositions is all less than 1.27%, shows that instrument precision is good.
table 4precision test result
2.2.3 stability test
The preparation of need testing solution takes compound recipe XUEZHINING two parts according to prescription, adds 25 DEG C of full Heshui solution of the water of 10 times amount, β-CD respectively, soaks 1h, backflow 1h, filtered while hot, and concentrating under reduced pressure obtains extractum; Extractum 40 DEG C of vacuum dryings porphyrize obtains XUEZHINING water extract powder, β-CD water solution extract powder.Take water extract powder, β-CD water solution extract powder 0.05g respectively, add methanol 5mL, weigh, ultrasonic 30min, puts and supply weightlessness to room temperature, shakes up, solution centrifugal (12000rpm, get supernatant 10min), thin up 1 times filters (0.22 μm) afterwards, subsequent filtrate sample introduction.
Respectively at 0,2,4,6,8,10,12h sample introduction, the peak area measuring each composition investigates the stability of need testing solution, calculates RSD value.Result shows that the RSD of 5 compositions is all less than 2.44%, and it is basicly stable that need testing solution room temperature places 24h.
2.2.4 replica test
By the parallel preparation of method 6 parts of need testing solutions under " need testing solution preparation " item under 2.2.3 stability test, measure peak area by chromatographic condition sample introduction under " 2.1 " item, calculate RSD value, result of calculation is shown in
table 5, each composition RSD value is all less than 2.56%, shows that test repeatability is good.
table 5replica test result (μ g/g, n=6)
2.2.5 average recovery test
Compound recipe XUEZHINING 6 parts is taken according to prescription, 25 DEG C of full Heshui solution of β-CD respectively, soak 1h, backflow 1h, filtered while hot, be cooled to and get 1mL after room temperature measures volume and be placed in 10mL volumetric flask, with pure methanol dilution, ultrasonic 30min, the centrifugal (12000rpm of diluent, get supernatant liquid filtering (0.22 μm) 10min), subsequent filtrate is sample introduction analysis respectively.After recording sample size, get 6 parts of each 0.5mL of extracting solution respectively and be placed in 10mL volumetric flask, add appropriate reference substance solution, with pure methanol dilution, ultrasonic 30min, gets supernatant liquid filtering (0.22 μm) after diluent centrifugal (12000rpm, 10min), subsequent filtrate respectively sample introduction analysis measures average recovery, the results are shown in
table 6.
table 6average recovery result of the test
The assay of each index components in 2.3 medical materials
2.3.1 the preparation of need testing solution
The mensuration of rubrofusarin O-gentibioside takes Semen Cassiae sample (crossing No. three sieves) 0.05g, accurately weighed, puts in tool plug conical flask, precision adds methanol 25mL, weighs, reflux, extract, 2h, put to room temperature, then weigh, supply weightlessness, shake up, leave standstill, supernatant filtering with microporous membrane, gets subsequent filtrate, be need testing solution, for subsequent use.
The mensuration of stilbene glucoside takes Radix Polygoni Multiflori Preparata sample (crossing No. four sieves) 0.2g, accurately weighed, puts in tool plug conical flask, precision adds Diluted Alcohol 25mL, weighed weight, reflux 30min, let cool, more weighed weight, supply weightlessness with Diluted Alcohol, shake up, leave standstill, supernatant filtering with microporous membrane, get subsequent filtrate 1mL to 10mL volumetric flask, with Diluted Alcohol standardize solution, be need testing solution, for subsequent use.
The assay of emodin in Semen Cassiae takes Semen Cassiae sample (crossing No. three sieves) 0.5g, and accurately weighed, precision adds 70% ethanol 50mL, weigh, reflux, extract, 2h, puts to room temperature, weigh again, supply weightlessness, shake up, leave standstill, supernatant filtering with microporous membrane, get subsequent filtrate, be need testing solution, for subsequent use.
The assay of emodin in Radix Polygoni Multiflori Preparata takes Radix Polygoni Multiflori Preparata sample (crossing No. four sieves) 1g, accurately weighed, puts in tool plug conical flask, precision adds methanol 50mL, weighed weight, reflux 1h, let cool, more weighed weight, supply weightlessness with methanol, shake up, leave standstill, supernatant filtering with microporous membrane, precision measures in subsequent filtrate 1mL to 10mL volumetric flask with methanol constant volume, be need testing solution, for subsequent use.
The mensuration of nuciferine takes Folium Nelumbinis sample (coarse powder) 0.5g, accurately weighed, puts in tool plug conical flask, precision adds methanol 50mL, weighed weight, reflux 2.5h, let cool, more weighed weight, supply weightlessness with methanol, shake up, filter, subsequent filtrate is after methanol dilution 10 times, precision measures diluent 5mL, puts in 10mL measuring bottle, adds water to scale, shake up, be need testing solution, for subsequent use.
Prepared by Quercetin need testing solution: take Folium Nelumbinis sample (coarse powder) 2g, accurately weighed, puts in tool plug conical flask, precision adds 60% ethanol 40mL, weighed weight, reflux 1h, let cool, more weighed weight, supply weightlessness, shake up, leave standstill, supernatant filtering with microporous membrane, precision measures in subsequent filtrate 1mL to 10mL volumetric flask with 60% ethanol standardize solution, be need testing solution, for subsequent use.
2.3.2 measurement result
The assay result of each composition in medical material
as table 7shown in.
table 7assay result
2.3.3 the computational methods of each constituents extraction rate of transform
C is compound extract concentration (mgmL
-1); V is extracting liquid volume (mL); Medical material actual mass (g) that m claims when being compound recipe extraction; W is this component content (mgg in medical material that originates in compound recipe
-1).
Note: when the extraction rate of transform of emodin calculates, m is the Semen Cassiae that claims when extracting of compound recipe and Radix Polygoni Multiflori Preparata quality (g) sum, and w is the content (mgg of emodin in Semen Cassiae and Radix Polygoni Multiflori Preparata
-1) sum.
2.4.1 solid-liquid ratio
Four Chinese medicine material 3 parts is taken respectively by compound recipe amount, add the β-CD saturated solution (25 DEG C) that solid-liquid ratio is 10 times, 20 times, 30 times respectively, after soaking 1h, backflow 1h, extracting solution filtered while hot, be cooled to and pipette 1mL after room temperature measures volume and be placed in 10mL volumetric flask, with pure methanol dilution standardize solution, ultrasonic 30min, the centrifugal (12000rpm of diluent, get supernatant liquid filtering (0.22 μm) 10min), subsequent filtrate sample introduction is analyzed.Calculate each constituents extraction rate of transform (
table 8), take solid-liquid ratio as abscissa, each constituents extraction rate of transform is that vertical coordinate is done
figure,
as Fig. 2 A,
fig. 2 B,
fig. 2 C,
fig. 2 D, and
fig. 2 Eshown in,
fig. 2 A,
fig. 2 B,
fig. 2 C,
fig. 2 D, and
fig. 2 Ebe respectively the investigation result of different feed liquid than lower five kinds of compositions of compound recipe XUEZHINING of the present invention and β-CD solution
figure, wherein,
fig. 2 Afor different feed liquid is than the extraction rate of transform of lower rubrofusarin O-gentibioside
figure,
fig. 2 Bfor different feed liquid is than the extraction rate of transform of lower stilbene glucoside
figure,
fig. 2 Cfor different feed liquid is than the extraction rate of transform of lower emodin
figure,
fig. 2 Dfor different feed liquid is than the extraction rate of transform of lower nuciferine
figure,
fig. 2 Efor different feed liquid is than the extraction rate of transform of lower Quercetin
figure; Rubrofusarin O-gentibioside, stilbene glucoside, nuciferine extract the rate of transform and obviously do not change in 20 times of solid-liquid ratios with 30 times, the extraction rate of transform of Quercetin increases with the increase of solid-liquid ratio, and the emodin extraction rate of transform is maximum in 20 times amount, consider the factor such as economy and post processing, when carrying out other single factor exploration, choose 20 times of solid-liquid ratios.
table 8feed liquid measurement result
2.4.2 the side of extraction
method is investigated
Four Chinese medicine material 3 parts is taken respectively by compound recipe amount, Extraction solvent is β-CD saturated solution (25 DEG C), solid-liquid ratio is 20:1, after soaking 1h, adopt hot dipping to extract (80 DEG C) 3h, supersound extraction 1h respectively, backflow 1h extracts, extracting liquid filtering, be cooled to and pipette 1mL after room temperature measures volume and be placed in 10mL volumetric flask, with pure methanol dilution standardize solution, ultrasonic 30min, get supernatant liquid filtering (0.22 μm) after diluent centrifugal (12000rpm, 10min), subsequent filtrate sample introduction is analyzed.Calculate each constituents extraction rate of transform (
table 9), the extraction rate of transform of each composition of contrast Different Extraction Method,
as Fig. 3shown in, wherein,
fig. 3in 1 identification post body display hot dipping extract the extraction rate of transform of five kinds of compositions in (80 DEG C) method, the extraction rate of transform of five kinds of compositions in 2 identification post body display ultrasonic extracting methods, the extraction rate of transform of five kinds of compositions in 3 identification post body display reflux extraction method, consider each composition result, reflowing result is better, therefore selects heating reflux method to extract compound recipe.
table 9also show this result.
table 9dNA extration result
2.4.3 extraction time is investigated
Four Chinese medicine material is taken by compound recipe amount, Extraction solvent is CD saturated solution (25 DEG C), and solid-liquid ratio is 20:1, after soaking 1h, reflux 0.5 respectively, 1,1.5,2,3h extracts, extracting solution filtered while hot, is cooled to and pipettes 1mL after room temperature measures volume and be placed in 10mL volumetric flask, with pure methanol dilution standardize solution, ultrasonic 30min, get supernatant liquid filtering (0.22 μm) after diluent centrifugal (12000rpm, 10min), subsequent filtrate sample introduction is analyzed.Calculate each constituents extraction rate of transform (
table 10), take extraction time as abscissa, each constituents extraction rate of transform is vertical coordinate,
as Fig. 4 A,
fig. 4 B,
fig. 4 C,
fig. 4 D, and
fig. 4 Eshown in,
fig. 4 A,
fig. 4 B,
fig. 4 C,
fig. 4 D, and
fig. 4 Ebe respectively in the present invention different extraction times lower five kinds of compositions investigation result
figure.Wherein,
fig. 4 Afor the extraction rate of transform of rubrofusarin O-gentibioside under different extraction time
figure,
fig. 4 Bfor the extraction rate of transform of stilbene glucoside under different extraction time
figure,
fig. 4 Cfor the extraction rate of transform of emodin under different extraction time
figure,
fig. 4 Dfor the extraction rate of transform of nuciferine under different extraction time
figure,
fig. 4 Efor the extraction rate of transform of Quercetin under different extraction time
figure, each constituents extraction rate of transform over time trend differs greatly, and needs further by orthogonal test overall merit.
table 10 extraction time investigated result
2.4.4 extraction time
Take four Chinese medicine material 3 parts by compound recipe amount, Extraction solvent is CD saturated solution (25 DEG C), and solid-liquid ratio is 20:1, and after soaking 1h, backflow 1h extracts, and extracts 1,2,3 time respectively, extracting solution filtered while hot, is cooled to the volume that room temperature measures extracting solution.Pipette 1mL extracting solution and be placed in 10mL volumetric flask, with pure methanol dilution standardize solution, ultrasonic 30min, gets supernatant liquid filtering (0.22 μm) after diluent centrifugal (12000rpm, 10min), and subsequent filtrate sample introduction is analyzed.Calculate each constituents extraction rate of transform (
table 11), take extraction time as abscissa, each constituents extraction rate of transform is vertical coordinate,
as Fig. 5 A,
fig. 5 B,
fig. 5 C,
fig. 5 D, and
fig. 5 Eshown in,
fig. 5 A,
fig. 5 B,
fig. 5 C,
fig. 5 D, and
fig. 5 Ebe respectively the investigation result of the lower five kinds of compositions of different extraction times in the present invention
figure.Wherein,
fig. 5 Afor the extraction rate of transform of rubrofusarin O-gentibioside under different extraction time
figure,
fig. 5 Bfor the extraction rate of transform of stilbene glucoside under different extraction time
figure,
fig. 5 Cfor the extraction rate of transform of emodin under different extraction time
figure,
fig. 5 Dfor the extraction rate of transform of nuciferine under different extraction time
figure,
fig. 5 Efor the extraction rate of transform of Quercetin under different extraction time
figure; Each constituents extraction rate of transform increases with extraction time and increases.
table 11 extraction time result
2.4.5 β-CD consumption
Take the some parts of four Chinese medicine material by compound recipe amount, press
table 1shown in 2, " β-CD addition and quality of medicinal material ratio/% " adds the β-CD of different quality respectively, and solid-liquid ratio is 20:1, and after soaking 1h, backflow 1h extracts, and extracting solution filtered while hot, is cooled to the volume that room temperature measures extracting solution.Pipette 1mL extracting solution and be placed in 10mL volumetric flask, with pure methanol dilution standardize solution, ultrasonic 30min, gets supernatant liquid filtering (0.22 μm) after diluent centrifugal (12000rpm, 10min), and subsequent filtrate sample introduction is analyzed.Calculate each constituents extraction rate of transform (
table 12), with " β-CD addition and quality of medicinal material ratio/% ", for abscissa, each constituents extraction rate of transform is vertical coordinate,
as Fig. 6 A,
fig. 6 B,
fig. 6 C,
fig. 6 D, and
fig. 6 Eshown in,
fig. 6 A,
fig. 6 B,
fig. 6 C,
fig. 6 D, and
fig. 6 Ebe respectively the investigation result of the lower five kinds of compositions of different beta-CD consumption in the present invention
figure.Wherein,
fig. 6 Afor the extraction rate of transform of rubrofusarin O-gentibioside under different beta-CD consumption
figure,
fig. 6 Bfor the extraction rate of transform of stilbene glucoside under different beta-CD consumption
figure,
fig. 6 Cfor the extraction rate of transform of emodin under different beta-CD consumption
figure,
fig. 6 Dfor the extraction rate of transform of nuciferine under different beta-CD consumption
figure,
fig. 6 Efor the extraction rate of transform of Quercetin under different beta-CD consumption
figure, each constituents extraction rate of transform presents different trend with the increase of β-CD consumption, and the overall evaluation for compound recipe XUEZHINING extraction process also need further by optimization of orthogonal test β-CD consumption.
table 12 β-CD consumptions investigate result
2.5 orthogonal test
2.5.1 Orthogonal Experiment and Design
Design four factor three horizontal quadrature tests according to single factor exploration result each under " 2.4 " item, choose β-CD consumption, extraction time, extraction time and solid-liquid ratio four factors, each factor chooses three levels, L9 (3
4) orthogonal design is shown in
table 13.
table 13 orthogonal tests
table
Take four Chinese medicine material 9 parts by compound recipe amount, press
table 1respectively it is extracted shown in 3, extracting solution filtered while hot, be cooled to the volume that room temperature measures extracting solution.Pipette 1mL extracting solution and be placed in 10mL volumetric flask, with pure methanol dilution standardize solution, ultrasonic 30min, centrifugal (the 12000rpm of diluent, get supernatant liquid filtering (0.22 μm) 10min), subsequent filtrate sample introduction is analyzed, and calculates each constituents extraction rate of transform.After extracting solution is concentrated, be placed in the evaporating dish being dried to constant weight, water-soluble evaporate to dryness, is dried to constant weight, takes out, and puts in exsiccator and weighs after cooling, calculates yield of extract, the results are shown in
table 17 Hes
table 18.
2.5.2 the calculating of weight coefficient
This test adopts multi index evaluation method to evaluate orthogonal experiments, from the extraction rate of transform of rubrofusarin O-gentibioside, stilbene glucoside, emodin, nuciferine, Quercetin 5 compositions as evaluation index, adopt analytic hierarchy process (AHP) (AHP)
[50]determine the weight coefficient of each composition.
Set up Evaluation target tree β-CD complementary extraction compound recipe XUEZHINING extraction process evaluation objective to reflect by rubrofusarin O-gentibioside, stilbene glucoside, emodin, nuciferine, Quercetin 5 subgoals.
Form the relative importance comparing precedence matrix comparison object between two, and form comparator matrix between two, the precedence matrix of 5 target paired comparison is shown in
table 14, standards of grading are shown in
table 15.
table 145 target paired comparison judge precedence matrix
table 1the each level scoring of 5 goal tree
table
Calculate initial weight coefficient and press formula
calculate initial weight coefficient w '
i.
w′
2＝2.2679，w′
3＝0.9221，w′
4＝0.5743，w′
5＝0.3671。
Calculate normalized weight coefficient and press formula
calculate normalized weight coefficient.w
1＝2.2679/(2.267+2.267+0.9221+0.5743+0.3671)＝0.3544，w
2＝0.3544，w
3＝0.1441，w
4＝0.0898，w
5＝0.0574。
Calculate the random consistent ratio of weight coefficient and calculate random Consistency Ratio by formula CR=CI/RI,
(
(
m is the secondary number of targets by inspection level, m=5), search corresponding Aver-age Random Consistency Index RI (random index), see
table 16.
λ
max=1/5 [(1 × 0.3544+1 × 0.3544+3 × 0.1441+4 × 0.0898+5 × 0.0574)/0.3544+ (1 × 0.3544+1 × 0.3544+3 × 0.1441+4 × 0.0898+5 × 0.0574)/0.3544+ (1/3 × 0.3544+1/3 × 0.3544+1 × 0.1441+2 × 0.0898+3 × 0.0574)/0.1441+ (1/4 × 0.3544+1/4 × 0.3544+1/2 × 0.1441+1 × 0.0898+2 × 0.0574)/0.0898+ (1/5 × 0.3544+1/5 × 0.3544+1/3 × 0.1441+1/2 × 0.0898+1 × 0.0574)/0.0574]=5.0620, CI=(5.0620-5)/(5-1)=0.0155, CR=0.0155/1.12=0.0138, CR<0.1, therefore think that judgment matrix has satisfied concordance, show that weight coefficient is rationally effective, can be used in the preferred comprehensive grading of next step extraction process.
table 16 Aver-age Random Consistency Index RI
table
2.5.3 orthogonal experiments analysis and demonstration test
table 17 orthogonal experiments
Note: comprehensive grading=rubrofusarin O-gentibioside scoring+stilbene glucoside scoring+emodin scoring+nuciferine scoring+Quercetin scoring; Each component scores=this constituents extraction rate of transform/maximum extracted rate of transform × weight coefficient × 100.
table 18 intuitive analysiss
table
table 19 variance analyses
table
From intuitive analysis, it is C>B>D>A that the extreme difference size of comprehensive grading number shows each factor effect primary and secondary, and optimised process is A
3b
3c
3d
3, the results of analysis of variance shows, extraction time and extraction time are significance influence factor.Comprehensive analysis, considers that significance influence factor and assisted extraction material too much, should not determine that optimised process is combined as A
1b
3c
3d
3, namely adopt β-CD addition to account for compound recipe medical material total amount 5%, 25 times amount reflux, extract, 3 times, each 2h.By fixed optimal extract process, repeated trials 3 times.Adopt water as Extraction solvent, other extraction processes remain unchanged, parallel test 3 times, contrast extraction with aqueous solution and the complementary extraction of β-CD between difference (
table 20).
as Fig. 7shown in,
fig. 7for the comparison of the extraction rate of transform of five kinds of compositions in the extraction with aqueous solution in the present invention and β-CD extracting method
figure,
in figure* represents there is significant difference, P<0.01 compared with water extraction,
fig. 7middle A shows the extraction rate of transform of five kinds of compositions in aqueous extraction process,
fig. 7middle B shows the extraction rate of transform of five kinds of compositions in β-CD extracting method.
table 20 confirmatory experiment result
Result shows, β-CD solution makes the extraction rate of transform significance of 5 kinds of index compositions in compound recipe XUEZHINING improve, but it is different to the influence degree of variety classes compound, wherein affect larger on stilbene glucoside, the emodin extraction rate of transform, the extraction rate of transform for rubrofusarin-6-O-β-D-O-gentibioside, Quercetin has a certain impact, then more weak on the extraction rate of transform impact of nuciferine.
By establishing the optimised process of β-CD complementary extraction Chinese medicine compound XUEZHINING to single factor exploration and orthogonal test, extract compound recipe XUEZHINING with β-CD solution and aqueous solution respectively with same process, the extraction rate of transform of 5 index components all has significance to improve.Compared with traditional water extraction, β-CD has significant complementary extraction effect to 5 index components, in the extraction process to compound recipe XUEZHINING, have using value.
3. conclusion and discussion
3.1 paste-forming rates are also the important evaluation indexes examining or check technological level in Study on extraction, it has important references for follow-up preparation research and is worth, within the specific limits, paste-forming rate high meaning extracts fully, but it is too high, illustrate that extracting method does not have specific aim, while extraction active component, also add the extracted amount of impurity, and be unfavorable for preparation.Using paste-forming rate as reference index in this test,
as table 1shown in 7, the paste-forming rate of No. 3 extraction processes is comparatively moderate in 9 groups of experiments, considers the weighted scoring of 5 index components, determines that optimised process is combined as A
1b
3c
3d
3, namely adopt β-CD addition to account for compound recipe medical material total amount 5%, 25 times amount reflux, extract, 3 times, each 2h.β-CD complementary extraction gained paste-forming rate contrast extraction with aqueous solution increases (
table 20), illustrate that β-CD entirety improves the extraction rate of transform of the active component of compound recipe XUEZHINING.
3.2 β-CD assisted extraction all can make in compound recipe XUEZHINING 5 index components extraction rates of transform have the raising of significance relative to water extraction, can illustrate that β-CD has different selective extraction abilities for each composition to the difference of each constituents extraction rate of transform influence degree, one of its reason is that the difference of its structure makes β-CD have different Binding abilities to them, such as: the phenyl ring being connected with a hydroxyl in stilbene glucoside easily enters in β-CD cavity, hydroxyl wherein can form hydrogen bond in β-CD cavity, be conducive to clathration, and nuciferine is a kind of aporphine alkaloids, in structure, the phenyl ring of non-chord chain is easier to enter into β-CD cavity, but methoxyl group causes structure steric hindrance to this enclose, be unfavorable for the formation of clathrate, thus the extraction rate of transform impact of β-CD on nuciferine is comparatively faint.For the reason that research β-CD is different to each composition selective extraction ability, inquire in the Inclusion constant at β-CD and each composition etc.
The present invention also determines the Inclusion constant of 5 index components and β-CD respectively, have studied β-CD to the good composition of water solublity (rubrofusarin-6-O-β-D-O-gentibioside, stilbene glucoside) the impact of stability, and the composition (emodin that water solublity is poor, nuciferine and Quercetin) the impact of dissolubility, result display β-CD and 5 index components generation clathrations, Host-guest ratio is 1:1, infer that its assisted extraction mechanism of action for each composition is β-CD and each composition generation clathration, add the dissolubility of slightly water-soluble composition at water on the one hand, thus the concentration of each composition in extracting solution in increase leaching process, improve the stability of labile element on the other hand, decrease the loss that each composition produces because degraded occurs in the effects such as high temperature in leaching process, and β-CD is that they are different from the Binding ability of different types of structure compound to one of different reason of different compound selective extraction ability.
In sum, β-CD by with 5 index components generation clathrations, add its dissolubility, improve stability, thus the extraction rate of transform that improve 5 index components of significance, illustrate that it can active component in complementary extraction herbal mixture compound recipe, the application in compound extraction technics has the value of research further.
Each composition Inclusion constant measurement result
as table 2shown in 1, wherein emodin poorly water-soluble, the Inclusion constant of itself and β-CD cannot be measured by two counting backward technique, thus the method for phase solubility is adopted, for making the Inclusion constant tool comparability measured between each composition, adopt two counting backward technique and Phase solubility method to measure the Inclusion constant of Quercetin simultaneously, though measurement result shows two kinds of assay methods and records result and have difference, but still be in the same order of magnitude, illustrate that Phase solubility method records the two counting backward technique of emodin Inclusion constant and other 4 compositions and records result and have certain comparability.
table 21 Inclusion constant measurement result
From
table 2can find out in 1, stilbene glucoside and β-cdinclusion constant maximum, rubrofusarin O-gentibioside, emodin and Quercetin take second place, and nuciferine is less,
as table 2shown in 0; β-CD records result for the selective extraction ability of each composition and Inclusion constant and matches; infer accordingly; β-CD is comparatively strong for the selective extraction ability of the larger material of Inclusion constant, and complementary extraction effect is more obvious, and prompting β-CD is obvious for the chemical composition stronger with its Binding ability complementary extraction effect; not only can be applicable to extracting technique of Chinese medicine; also can be applicable to the preparation of some composition reference substance, the use of organic solvent can be reduced, thus preserve the ecological environment.
β-CD can increase rubrofusarin O-gentibioside and the stability of stilbene glucoside in high temperature (90 DEG C) environment, illustrate that β-CD can by increasing ingredient stability in leaching process on the one hand, reduce the degraded that it occurs in hot conditions, thus the extraction that improve the two moves rate; On the other hand after the complementary extraction of β-CD, in extract, each ingredient stability is improved to some extent, and reduces its loss in preservation process, thus adds medical material utilization rate.
The solubilization result of study of (emodin, nuciferine and Quercetin) is divided to show to shipwreck melt into, β-CD all has certain solubilization to emodin, nuciferine and Quercetin, can infer, β-CD is by improving its dissolubility in water after forming clathrate with compound, the dissolution equilibrium of this compound is moved right, makes it easilier shift to extracting solution from medical material.
Embodiment 2
The crude drug of compound recipe XUEZHINING comprises Semen Cassiae, Radix Polygoni Multiflori Preparata, Folium Nelumbinis and Fructus Crataegi, the part by weight of described Semen Cassiae, Radix Polygoni Multiflori Preparata, Folium Nelumbinis and Fructus Crataegi is 3:2:1.5:1, and active component comprises rubrofusarin-6-O-β-D-O-gentibioside, stilbene glucoside, emodin, nuciferine and Quercetin.
In beta-schardinger dextrin-solution, the consumption of beta-schardinger dextrin-account for the crude drug gross weight of described compound recipe XUEZHINING 5%, be the EDTA of 0.08mg/mL containing mass body volume concentrations, its pH is 2.5 ~ 3.0, and the crude drug of compound recipe XUEZHINING and the solid-liquid ratio of beta-schardinger dextrin-solution are 1:25.
The method extracting active component from the crude drug of compound recipe XUEZHINING comprises the steps: that being pulverized by crude drug is 100 object granules, join again in beta-schardinger dextrin-solution afterwards and soak 1h, afterwards 3 times are extracted to the mixed-liquor return of described crude drug and beta-schardinger dextrin-solution, each return time is 2h, wherein, the 1st time of reflux, extract, certain time through four-stage and under each stage successively, first first stage refluxes to the liquid of 70% of the described mixeding liquid volume of described crude drug and beta-schardinger dextrin-solution, afterwards second, third and fourth stage added 1/3 of residual mixed liquor volume more respectively and refluxes.In reflux, extract, the described first stage continues 40min, described second and the phase III respectively continue 20min, described fourth stage continues 40min.All add again when previous mixed liquor is cooled to room temperature with during mixed liquor between each stage.
After last backflow completes, extracting solution filtered while hot, is cooled to the volume that room temperature measures extracting solution.Pipette 1mL extracting solution and be placed in 10mL volumetric flask, with pure methanol dilution standardize solution, ultrasonic 30min, centrifugal (the 12000rpm of diluent, get supernatant liquid filtering (0.22 μm) 10min), subsequent filtrate sample introduction is analyzed, and calculates each constituents extraction rate of transform.After extracting solution is concentrated, be placed in the evaporating dish being dried to constant weight, water-soluble evaporate to dryness, is dried to constant weight, takes out, and puts in exsiccator and weighs after cooling, calculates yield of extract, result
as table 2shown in 2.
table 22 each constituents extraction rates of transform
Scientific and reasonable extracting technique of Chinese medicine, the aspect such as continual exploitation, pharmacology's further investigation, form of Chinese drug development, raising tcm product production efficiency for Chinese medicine has important and profound significance.For the research of extracting technique of Chinese medicine, need according to Chinese crude drug feature, the difference extracting target component characteristic, the statistical method of choose reasonable process optimization, consider, hold the various factors affecting extraction efficiency comprehensively, the extraction efficiency of active component, active component is made to improve as far as possible, strengthen the controllability of extraction process, extracting technique of Chinese medicine is studied to efficient, controlled, energy saving direction development.
Although embodiment of the present invention are open as above, but it is not restricted to listed in description and embodiment utilization, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore do not deviating under the general concept that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and describe
figureexample.
Claims (10)
1. one kind is extracted the method for active component from the crude drug of compound recipe XUEZHINING, it is characterized in that, comprise the steps: the crude drug of compound recipe XUEZHINING to join in beta-schardinger dextrin-solution to soak 1h, afterwards the mixed-liquor return of described crude drug and beta-schardinger dextrin-solution is extracted 1 ~ 3 time, each return time is 1 ~ 2h, wherein, the consumption of beta-schardinger dextrin-accounts for 5% ~ 15% of the crude drug gross weight of described compound recipe XUEZHINING, and the crude drug of described compound recipe XUEZHINING and the solid-liquid ratio of described beta-schardinger dextrin-solution are 1:25 ~ 1:15.
2. from the crude drug of compound recipe XUEZHINING, extract the method for active component as claimed in claim 1, it is characterized in that, the consumption of beta-schardinger dextrin-accounts for 5% of the crude drug gross weight of described compound recipe XUEZHINING.
3. from the crude drug of compound recipe XUEZHINING, extract the method for active component as claimed in claim 1, it is characterized in that, the crude drug of described compound recipe XUEZHINING and the solid-liquid ratio of described beta-schardinger dextrin-solution are 1:25.
4. from the crude drug of compound recipe XUEZHINING, extract the method for active component as claimed in claim 1, it is characterized in that, the crude drug of compound recipe XUEZHINING is joined in beta-schardinger dextrin-solution and soaks 1h, afterwards heating and refluxing extraction 3 times.
5. from the crude drug of compound recipe XUEZHINING, extract the method for active component as claimed in claim 1, it is characterized in that, in described reflux, each return time is 2h.
6. the method extracting active component from the crude drug of compound recipe XUEZHINING as described in as arbitrary in claim 1 to 5, it is characterized in that, the crude drug of described compound recipe XUEZHINING comprises Semen Cassiae, Radix Polygoni Multiflori Preparata, Folium Nelumbinis and Fructus Crataegi, and the part by weight of described Semen Cassiae, Radix Polygoni Multiflori Preparata, Folium Nelumbinis and Fructus Crataegi is 3:2:1.5:1.
7. from the crude drug of compound recipe XUEZHINING, extract the method for active component as claimed in claim 6, it is characterized in that, also containing mass body volume concentrations in described beta-schardinger dextrin-solution is the EDTA of 0.08mg/mL, and the pH of described beta-schardinger dextrin-solution is 2.5 ~ 3.0.
8. from the crude drug of compound recipe XUEZHINING, extract the method for active component as claimed in claim 1, it is characterized in that, first being pulverized by the crude drug of compound recipe XUEZHINING is 100 object granules, joins in beta-schardinger dextrin-solution afterwards again and soaks.
9. from the crude drug of compound recipe XUEZHINING, extract the method for active component as claimed in claim 5, it is characterized in that, the 1st time of reflux, extract, certain time through four-stage and under each stage successively, first first stage refluxes to the liquid of 70% of the described mixeding liquid volume of described crude drug and beta-schardinger dextrin-solution, afterwards second, third and fourth stage added 1/3 of residual mixed liquor volume more respectively and refluxes, wherein, the described first stage continues 40min, described second and the phase III respectively continue 20min, described fourth stage continues 40min.
10. from the crude drug of compound recipe XUEZHINING, extract the method for active component as claimed in claim 1, it is characterized in that, described active component comprises rubrofusarin-6-O-β-D-O-gentibioside, stilbene glucoside, emodin, nuciferine and Quercetin.
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