CN102813687A - Use of ligustilide in preparing anti-thrombotic medicines - Google Patents
Use of ligustilide in preparing anti-thrombotic medicines Download PDFInfo
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Abstract
The invention relates to use of ligustilide in preparing anti-thrombotic medicines, in particular to a rhizoma ligustici wallichii extract. The rhizoma ligustici wallichii extract contains 30-90 percent of ligustilide. The extract is prepared by adopting a method comprising the following steps of: crushing a rhizoma ligustici wallichii medicinal material; then, soaking by using 70-99 percent of alcohol (for example 75-98 percent), and performing reflux extraction for 1-4 times; merging extracting solutions; concentrating; extracting by using petroleum ether; recovering solvents from the merged extracting solutions until dry to obtain petroleum ether extracting extractum; adding part of petroleum ether extracting extractum to positive-phase silica gel and mixing to exceed a positive-phase silica gel column; performing elution by taking the petroleum ether and an ethyl acetate solution as eluents; collecting the eluents; concentrating to obtain the rhizoma ligustici wallichii extract, wherein the volume ratio of the petroleum ether to the ethyl acetate solution is 50:(0.5-5) [for example 50:(0.5-3)].
Description
Technical field
The invention belongs to the Chemistry for Chinese Traditional Medicine field, relate in particular to a kind of active component that from Rhizoma Chuanxiong, extracts and preparation method thereof, and the purposes of this component in the preparation antithrombotic reagent.
Background technology
Thrombosis (thrombosis) is meant in heart and lumen of vessels, blood solidify or blood in the sticking mutually collection of some visible component, form the process of solid matter piece.Under pathologic condition, the vessel lumen that thrombosis causes is blocked and other influences, can cause serious even fatal harm to body, becomes the important paathogenic factor of cardiovascular and cerebrovascular diseases such as myocardial infarction, apoplexy, DVT, pulmonary infarction.
The tunica intima damage is one of thrombotic major incentive.Vascular endothelial cell is thrombin, a hematoblastic unicellular thin film in subcutaneous connective tissue and the blood in one deck is separated, and has anticoagulant, the sticking function that collects of antiplatelet.But when endotheliocyte is impaired, in basement membrane collagen, fibril property collagen, elastin laminin in the subcutaneous connective tissue intensive blood coagulation enhancing effect is all arranged, cause the sticking collection of platelet to form thrombosis.What in triggering coagulation process, play the role of a nucleus is hematoblastic activation.Hematoblastic material be can activate and collagen, thrombin, ADP etc. comprised; Behind endothelial injury; At first activating hematoblastic is the collagen that contacts with platelet; Continue after the blood coagulation chain reflex be activated and produced thrombin, and platelet is activated unceasingly and constantly disengages ADP and thromboxane A2, what come with blood flow is that platelet constantly is activated in the part.Therefore, the blocking platelet activation and prevent endothelial injury be the prevention and the treatment thrombotic disease effective way.
Antithrombotic therapy is the effective means that apoplexy, coronary artery thrombosis cause disease prevention such as myocardial infarction, thromboangiitis obliterans and treatment always.Antithrombotic reagent commonly used mainly comprises three types, and promptly anticoagulant, antiplatelet drug and thrombolytic medicine are representative with heparin, aspirin and urokinase respectively.Modern pharmacological research shows; Some blood-activating stasis-removing kind Chinese medicines such as decoction for removing blood stasis etc. can improve hemorheological properties; Reduce and hematoblasticly stick and assemble; Reduce hematoblastic surface activity, simultaneously through a plurality of approach preventions and treatment thrombotic disease such as anticoagulant, the impaired endotheliocytes of protection.Therefore, seek from Chinese medicine and have antiplatelet aggregation and become the new source of developing antithrombotic reagent with the active active component of protection of ecs.
Rhizoma Chuanxiong is the samphire Rhizoma Chuanxiong
Ligusticum chuanxiongHort. dry rhizome, its nature and flavor are hot, temperature.Return liver, gallbladder, pericardium channel.The blood circulation promoting and blood stasis dispelling action range, the suitable various diseases of stagnation of blood stasis; Wind-expelling pain-stopping, effectiveness is excellent, can control diseases such as wind syndrome of head headache, rheumatic arthralgia.Modern pharmacology research shows; Rhizoma Chuanxiong extract has a dose-dependent inhibition effect to guinea-pig heart is dirty; Leave one's post rat or guinea pig heart all had the effect of significant increase coronary flow; Its main active ligustrazine can be expanded the induced lung blood vessel, suppresses hypoxic pulmonary vascular contractile response and right ventricular hypertrophy.In addition, Rhizoma Chuanxiong also has central nervous system's inhibitory action, movable inhibited to animal brain, and medulla oblongata respiratory center, vasomotor center and spinal reflex maincenter are had excitation.The main compound ligustrazine can suppress thromboxane A2 (TXA in the Rhizoma Chuanxiong
2) synthetic, its effect and TXA
2The synthetase inhibitors effect is similar.But research at present mostly concentrates on compositions such as ligustrazine and ferulic acid, whether has antithrombotic acitivity and mechanism of action it be unclear that for the chuanxiong lactone kind component.
Summary of the invention
The purpose of this invention is to provide a kind of chuanxiong rhizome effective ingredient, this active component mainly contains ligustilide, and content is 30 ~ 90%.
Another object of the present invention provides the method for preparing of this chuanxiong rhizome effective ingredient, realizes through following steps: with adding 20% ~ 90% soak with ethanol after the Rhizoma Chuanxiong pulverizing medicinal materials 5 ~ 12 hours, heating and refluxing extraction 0.8 ~ 1.2 hour; Extract 1 ~ 3 time; Merging filtrate gets extracting solution, and extracting solution is used petroleum ether extraction, extract is concentrated the back with normal phase silicagel column it is carried out purification; The petroleum ether and the ethyl acetate that with the volume ratio are 50:1 are eluant, collect to obtain active component after eluent concentrates.
A further object of the present invention provides the application of this chuanxiong rhizome effective ingredient in the preparation antithrombotic reagent.
First aspect present invention provides a kind of Rhizoma Chuanxiong extract, wherein contains 30 ~ 90% ligustilide.
According to the Rhizoma Chuanxiong extract of first aspect present invention, wherein contain the ligustilide of 80 ~ 97% (for example 85%-95%).
Rhizoma Chuanxiong extract according to first aspect present invention; It prepares through following method: after the Rhizoma Chuanxiong pulverizing medicinal materials, soak and reflux, extract, 1-4 time merge extractive liquid, with 70% ~ 99% ethanol (for example 75% ~ 98%); Concentrate; Use petroleum ether extraction, the extract that merges is reclaimed solvent to doing, get petroleum ether extraction extractum; Getting petroleum ether extraction part extractum, add and cross normal phase silicagel column after purification on normal-phase silica gel is mixed appearance, is that the petroleum ether and the ethyl acetate solution of 50:0.5 ~ 5 (for example 50:0.5 ~ 3) is that eluant carries out eluting with the volume ratio, collects eluent, concentrates, and promptly gets.
According to the Rhizoma Chuanxiong extract of first aspect present invention, it prepares through following method: with adding 20% ~ 90% soak with ethanol after the Rhizoma Chuanxiong pulverizing medicinal materials 5 ~ 12 hours, heating and refluxing extraction 0.8 ~ 1.2 hour; Extract 1 ~ 3 time; Merging filtrate gets extracting solution, and extracting solution is used petroleum ether extraction, extract is concentrated the back with normal phase silicagel column it is carried out purification; The petroleum ether and the ethyl acetate that with the volume ratio are 50:1 are eluant, collect to obtain extract after eluent concentrates.
Rhizoma Chuanxiong extract according to first aspect present invention; It prepares through following method: after 1000g Rhizoma Chuanxiong pulverizing medicinal materials, add 4000ml 95% soak with ethanol and spend the night reflux, extract, 2 hours; Adding 4000ml again extracts 3 times with 95% alcohol heating reflux; Each 2h, merge extractive liquid, is concentrated into density 1.08; Concentrated solution added in the 500ml water be dispersed into suspension, add the 500ml petroleum ether extraction 3 times, combining extraction liquid reclaims solvent to doing.Getting petroleum ether extraction part extractum, add and cross normal phase silicagel column after purification on normal-phase silica gel is mixed appearance, is that petroleum ether and the ethyl acetate solution of 50:1 is that eluant carries out eluting with the volume ratio, collects eluent, after concentrating, promptly gets.
Second aspect present invention provides the method for preparing Rhizoma Chuanxiong extract; It may further comprise the steps: after the Rhizoma Chuanxiong pulverizing medicinal materials, soak and reflux, extract, 1-4 time merge extractive liquid, with 70% ~ 99% ethanol (for example 75% ~ 98%); Concentrate; Use petroleum ether extraction, the extract that merges is reclaimed solvent to doing, get petroleum ether extraction extractum; Getting petroleum ether extraction part extractum, add and cross normal phase silicagel column after purification on normal-phase silica gel is mixed appearance, is that the petroleum ether and the ethyl acetate solution of 50:0.5 ~ 5 (for example 50:0.5 ~ 3) is that eluant carries out eluting with the volume ratio, collects eluent, concentrates, and promptly gets.
According to the method for second aspect present invention, it may further comprise the steps: with adding 20% ~ 90% soak with ethanol after the Rhizoma Chuanxiong pulverizing medicinal materials 5 ~ 12 hours, heating and refluxing extraction 0.8 ~ 1.2 hour; Extract 1 ~ 3 time; Merging filtrate gets extracting solution, and extracting solution is used petroleum ether extraction, extract is concentrated the back with normal phase silicagel column it is carried out purification; The petroleum ether and the ethyl acetate that with the volume ratio are 50:1 are eluant, collect to obtain extract after eluent concentrates.
According to the method for second aspect present invention, it may further comprise the steps: after 1000g Rhizoma Chuanxiong pulverizing medicinal materials, add 4000ml 95% soak with ethanol and spend the night; Reflux, extract, 2 hours adds 4000ml again and extracts 3 times with 95% alcohol heating reflux, each 2h; Merge extractive liquid, is concentrated into density 1.08; Concentrated solution added in the 500ml water be dispersed into suspension, add the 500ml petroleum ether extraction 3 times, combining extraction liquid reclaims solvent to doing.Getting petroleum ether extraction part extractum, add and cross normal phase silicagel column after purification on normal-phase silica gel is mixed appearance, is that petroleum ether and the ethyl acetate solution of 50:1 is that eluant carries out eluting with the volume ratio, collects eluent, after concentrating, promptly gets.
According to the method for second aspect present invention, contain 30 ~ 90% ligustilide in its gained Rhizoma Chuanxiong extract.
According to the method for second aspect present invention, contain the ligustilide of 80 ~ 97% (for example 85%-95%) in its gained Rhizoma Chuanxiong extract.
Third aspect present invention provides the application of Rhizoma Chuanxiong extract in the preparation antithrombotic reagent of first aspect present invention.
Fourth aspect present invention provides a kind of pharmaceutical composition, comprising Rhizoma Chuanxiong extract and the pharmaceutically acceptable carrier or the excipient of first aspect present invention.
Chuanxiong rhizome effective ingredient of the present invention can be used as active site, adds drug excipient or the carrier accepted on the pharmaceutics, processes preparation according to the method for putting down in writing on the pharmaceutics.
The dosage form of said medicine comprises liquid preparation, solid preparation, capsule, soft gelatin capsule.Comprise injection, drip liquid, injectable powder, granule, tablet, electuary, powder, oral liquid, sugar coated tablet, film coated tablet, enteric coated tablet, capsule, hard capsule, soft capsule, suck agent, granule, pill, unguentum, sublimed preparation, spray, drop pill, disintegrating agent, oral cavity disintegration tablet, micropill etc.
In the present invention, term " chuanxiong rhizome effective ingredient " also can be described as " Rhizoma Chuanxiong component ", " Rhizoma Chuanxiong extract ", " cnidium lactone " etc., and these terms can exchange use.
Beneficial effect of the present invention is:
1. extraction and separation process of the present invention is simple, can obtain active component rapidly and accurately.
2. chuanxiong rhizome effective ingredient chemical constituent provided by the invention is simply clear and definite, on pharmacological research, is easier to illustrate its mechanism of action, is easier to the quality control of medicine aborning.
3. the present invention on model, has estimated the effect of chuanxiong lactone kind extract antiplatelet aggregation with protection inflammatory damage endotheliocyte first, obtains pharmacologically active preferably, for its purposes in the preparation antithrombotic reagent provides foundation.
Description of drawings
Fig. 1. be the efficient liquid phase chromatographic analysis figure of Rhizoma Chuanxiong extract of the present invention.
Fig. 2. the variable concentrations Rhizoma Chuanxiong extract is to the influence of the platelet aggregation of arachidonic acid-induction.
Fig. 3. the variable concentrations Rhizoma Chuanxiong extract is to the influence of the inductive platelet aggregation of ADP.
Fig. 4. the variable concentrations Rhizoma Chuanxiong extract is to the influence of collagen-induced platelet aggregation.
Fig. 5. the variable concentrations Rhizoma Chuanxiong extract is to the influence of TNF-α endothelial cell injury secretion adhesion factor.
Fig. 6. the influence that the variable concentrations Rhizoma Chuanxiong extract is expressed TNF-α endothelial cell injury nuclear factor NF-kB protein.
The specific embodiment
The present invention combines accompanying drawing and following embodiment further explain flesh and blood of the present invention, and this embodiment only is used to the present invention is described and is not limitation of the present invention.
The preparation of embodiment one chuanxiong rhizome effective ingredient
After 1000g Rhizoma Chuanxiong pulverizing medicinal materials, add 4000ml 95% soak with ethanol and spend the night, reflux, extract, 2 hours adds 4000ml again and extracts 3 times with 95% alcohol heating reflux, each 2h, merge extractive liquid, is concentrated into density 1.08.Concentrated solution added in the 500ml water be dispersed into suspension, add the 500ml petroleum ether extraction 3 times, combining extraction liquid reclaims solvent to doing.Get petroleum ether extraction part extractum; Adding and cross normal phase silicagel column after purification on normal-phase silica gel is mixed appearance, is that petroleum ether and the ethyl acetate solution of 50:1 is that eluant carries out eluting with the volume ratio, collects eluent; After concentrating, obtain weak yellow liquid 11.3g; Be Rhizoma Chuanxiong extract of the present invention, it also can be described as cnidium lactone in the present invention, and is used for hereinafter biological test example.
The analysis of embodiment two chuanxiong rhizome effective ingredients
Take by weighing Rhizoma Chuanxiong extract dissolving shown in embodiment 1, get and be transferred to brown liquid phase sample introduction bottle in right amount, be used for liquid-phase chromatographic analysis.
Analysis condition is following: Agilent 1100 type chromatograph of liquid, sample size 10 μ l; Flow velocity 1ml/min, 30 ℃ of column temperatures.The eluent gradient of chromatography is: 0 ~ 40min: water (0.1% formic acid): 70% ~ 20%, and acetonitrile: 30% ~ 80%; 40-50min: water (0.1% formic acid): 20% ~ 5%, acetonitrile: 80% ~ 95%; 50 ~ 55min: water (0.1% formic acid): 5%, acetonitrile: 95%; Detect wavelength 271nm.Analysis of spectra (abscissa be minute) as shown in Figure 1.Liquid-phase chromatographic analysis shows that Rhizoma Chuanxiong extract has 1 obvious chromatographic peak at 26.5min, identifies that after comparing with standard substance the chemical compound of this peak representative is a ligustilide.Analysis result shows that main component is a ligustilide in the extract of cnidium lactone, and its content is about 90%.Unexpectedly find; In embodiment 1; If be lower than 70% ethanol extraction with concentration, perhaps use petroleum ether to be eluant, the ethyl acetate deal is greater than 5 in the perhaps used eluant; When promptly 50 parts of petroleum ether and the ethyl acetate mixed liquor more than 5 parts were eluant, ligustilide acquisition amount was lower more than 30% than the acquisition amount of embodiment 1.With 75% above ethanol extraction, perhaps use petroleum ether: ethyl acetate is the mixed liquor of ratio of 50:0.5 ~ 3 during as eluent, ligustilide acquisition amount be embodiment 1 the acquisition amount 90% ~ 115%, and in the extract ligustilide content all 80 ~ 97%.
Embodiment three chuanxiong rhizome effective ingredient preparations
Get the chuanxiong rhizome effective ingredient 0.5g and 10.5g Polyethylene Glycol-6000 mix homogeneously of embodiment 1 gained, heating and melting moves in the drop pill drip irrigation behind the change material, and in ℃ liquid paraffin of medicine liquid droplet to 6 ~ 8, oil removing makes 400 of drop pill.
Embodiment Sichuan rhizome of chuanxiong active component preparation
Get the chuanxiong rhizome effective ingredient 0.5g of embodiment 1 gained, wear into fine powder, with about 1/3 starch mixing; Add the starch slurry mixing and process soft material, 16 mesh sieves are granulated, 70 ℃ of dryings; Dry granular is crossed 14 mesh sieve granulate, adds remaining starch (in advance 100-105 ℃ of drying) and the Pulvis Talci (light liquid petrolatum is sprayed on mixing in the Pulvis Talci) that is adsorbed with liquid Paraffin, again through 14 mesh sieves; Tabletting promptly gets.
Embodiment five extract of cnidium lactone platelet aggregation inhibitory activities are estimated
Platelet can be by multiple substance activating, still mainly through following approach: ADP approach, AA epoxidase approach and PAF (platelet activating factor) approach.These three approach are finally all through Ca in the increased platelets counts
2+Concentration and activate platelet.Exogenous collagen is mainly through the PAF approach.Present embodiment has been investigated like the influence of embodiment 1 gained cnidium lactone lactone extract to arachidonic acid (AA), adenosine diphosphate (ADP) (ADP) and the inductive platelet aggregation of collagen (COLL).
Adopt lignocaine cervical region local anesthesia New Zealand large ear rabbit, separate left carotid, common carotid artery adds 3.8% liquor sodii citratis anticoagulant after getting blood.The centrifugal 12min of 1000rmp, getting supernatant partly is platelet rich plasma (PRP), the centrifugal 10min of remainder 3000rmp, getting supernatant partly is platelet poor plasma (PPP).Use the Automatic Blood Cell Analyzer platelet Counting, adjust PRP with PPP, making platelet count is (3.0-5.0) * 10
9Individual/L.After inducing blood coagulation with dissimilar derivant ADP, AA and COLL; Measure the platelet aggregation inhibitory activity of extract of cnidium lactone (embodiment 1 gained) 0.05,0.1,0.2,0.4,0.6, under the 0.8mg/ml concentration; The clopidogrel of aspirin and 0.2mg/ml that adopts 0.05mg/ml is respectively measured platelet aggregation rate as positive drug with the 570-VS platelet aggregation instrument.
The result shows, after AA induces, assembles maximum agglutination rate average out to 68.04 rapidly.Under positive drug aspirin (Aspirin) is intervened, maximum agglutination rate significantly descend (
P<0.01).Embodiment 1 gained extract of cnidium lactone significantly descends at each dose groups PAR of 0.2-0.8 mg/ml at 0.05 mg/ml, 0.1 mg/ml dose groups and blank group no significant difference relatively, with blank group comparing difference significantly (
P<0.01), and be dose-dependence, shown in accompanying drawing 2 (control representes matched group among the figure, and aspirin representes the aspirin group).
Platelet rich plasma is assembled maximum agglutination rate average out to 48.15 rapidly after ADP induces.Under the intervention of positive drug clopidogrel, maximum agglutination rate significantly descend (
P<0.01).Embodiment 1 gained extract of cnidium lactone makes the inductive platelet aggregation rate of ADP significantly descend in the 0.6-1.4mg/ml concentration range, with blank group comparing difference significantly (
P<0.01), and be dose-dependence, (contr among the figure shown in accompanying drawing 3 ... The expression matched group, clopi ... Expression clopidogrel group).
Platelet rich plasma is assembled maximum agglutination rate average out to 70.77 rapidly through after collagen-induced.In aspirin and clopidogrel intervention, maximum agglutination rate significantly descend (
P<0.01).Cnidium lactone 0.05 mg/ml, 0.1 mg/ml dose groups and blank group be no significant difference relatively, and each dose groups PAR of 0.2-0.8 mg/ml significantly descends, with blank group comparing difference significantly (
P<0.01), and be dose-dependence, (control representes matched group among the figure, and aspirin representes aspirin group, clopido shown in accompanying drawing 4 ... Expression clopidogrel group).
The anti-endothelial cell damage activity rating of embodiment six extract of cnidium lactone
Investigate of the protective effect of embodiment 1 gained extract of cnidium lactone to the inflammatory damage endotheliocyte.In-vitro separation cultivating people's huve cell; TNF-α damages modeling; Simultaneously in addition the extract of cnidium lactone of variable concentrations (6.25,12.5,25ug/ml) is hatched 24h altogether; The content of adhesion molecule sICAM-1 and sVCAM-1 in ELISA (Elisa method) the mensuration cell culture fluid, Western blot measures NF-kB protein expression in the nucleus.The result shows that MTT result shows that TNF-α 10ng/ml can obviously cause cell injury, and the protection endotheliocyte of cnidium lactone dose dependent is avoided TNF-α damage; The expression of TNF-α significance ground rising endothelial cell adhesion molecule I CAM-1 and sVCAM-1 (p 0.01), the cnidium lactone high dose can reduce its expression in significance ground; Simultaneously Western blot result shows the protein expression of the minimizing Human umbilical vein endothelial cells NF-kB that cnidium lactone can dose dependent.Extract of cnidium lactone can protect endotheliocyte to avoid the damage of TNF-α, and its mechanism of action possibly be the protein expression through inhibition NF-κ B, and then the content of minimizing endothelial cell adhesion molecule I CAM-1 is relevant.The result sees Fig. 5, has shown that wherein the variable concentrations Rhizoma Chuanxiong extract representes people sICAM-1 and sVCAM-1 concentration (ug/ml) to the vertical coordinate that influences of TNF-α endothelial cell injury secretion adhesion factor.In addition, Fig. 6 has shown the influence that the variable concentrations Rhizoma Chuanxiong extract is expressed TNF-α endothelial cell injury nuclear factor NF-kB protein, and vertical coordinate representes that NF-κ B expresses (comparing with contrast) among the figure.
Claims (10)
1. a Rhizoma Chuanxiong extract wherein contains 30 ~ 90% ligustilide.
2. according to the Rhizoma Chuanxiong extract of claim 1, wherein contain 80 ~ 97% ligustilide.
3. according to the Rhizoma Chuanxiong extract of claim 1 or 2; It prepares through following method: after the Rhizoma Chuanxiong pulverizing medicinal materials, soak and reflux, extract, 1-4 time merge extractive liquid, with 70% ~ 99% ethanol (for example 75% ~ 98%); Concentrate; Use petroleum ether extraction, the extract that merges is reclaimed solvent to doing, get petroleum ether extraction extractum; Getting petroleum ether extraction part extractum, add and cross normal phase silicagel column after purification on normal-phase silica gel is mixed appearance, is that the petroleum ether and the ethyl acetate solution of 50:0.5 ~ 5 (for example 50:0.5 ~ 3) is that eluant carries out eluting with the volume ratio, collects eluent, concentrates, and promptly gets.
4. according to the Rhizoma Chuanxiong extract of claim 1 or 2, it prepares through following method: with adding 20% ~ 90% soak with ethanol after the Rhizoma Chuanxiong pulverizing medicinal materials 5 ~ 12 hours, heating and refluxing extraction 0.8 ~ 1.2 hour; Extract 1 ~ 3 time; Merging filtrate gets extracting solution, and extracting solution is used petroleum ether extraction, extract is concentrated the back with normal phase silicagel column it is carried out purification; The petroleum ether and the ethyl acetate that with the volume ratio are 50:1 are eluant, collect to obtain extract after eluent concentrates.
5. according to the Rhizoma Chuanxiong extract of claim 1 or 2; It prepares through following method: after 1000g Rhizoma Chuanxiong pulverizing medicinal materials, add 4000ml 95% soak with ethanol and spend the night reflux, extract, 2 hours; Adding 4000ml again extracts 3 times with 95% alcohol heating reflux; Each 2h, merge extractive liquid, is concentrated into density 1.08; Concentrated solution added in the 500ml water be dispersed into suspension, add the 500ml petroleum ether extraction 3 times, combining extraction liquid reclaims solvent to doing; Getting petroleum ether extraction part extractum, add and cross normal phase silicagel column after purification on normal-phase silica gel is mixed appearance, is that petroleum ether and the ethyl acetate solution of 50:1 is that eluant carries out eluting with the volume ratio, collects eluent, after concentrating, promptly gets.
6. prepare the method for Rhizoma Chuanxiong extract, it may further comprise the steps: after the Rhizoma Chuanxiong pulverizing medicinal materials, soak and reflux, extract, 1-4 time with 70% ~ 99% ethanol (for example 75% ~ 98%); Merge extractive liquid, concentrates, and uses petroleum ether extraction; The extract that merges is reclaimed solvent to doing, get petroleum ether extraction extractum; Getting petroleum ether extraction part extractum, add and cross normal phase silicagel column after purification on normal-phase silica gel is mixed appearance, is that the petroleum ether and the ethyl acetate solution of 50:0.5 ~ 5 (for example 50:0.5 ~ 3) is that eluant carries out eluting with the volume ratio, collects eluent, concentrates, and promptly gets.
7. according to the method for claim 6, it may further comprise the steps: with adding 20% ~ 90% soak with ethanol after the Rhizoma Chuanxiong pulverizing medicinal materials 5 ~ 12 hours, heating and refluxing extraction 0.8 ~ 1.2 hour; Extract 1 ~ 3 time; Merging filtrate gets extracting solution, and extracting solution is used petroleum ether extraction, extract is concentrated the back with normal phase silicagel column it is carried out purification; The petroleum ether and the ethyl acetate that with the volume ratio are 50:1 are eluant, collect to obtain extract after eluent concentrates.
8. according to the method for claim 6, it may further comprise the steps: after 1000g Rhizoma Chuanxiong pulverizing medicinal materials, add 4000ml 95% soak with ethanol and spend the night; Reflux, extract, 2 hours adds 4000ml again and extracts 3 times with 95% alcohol heating reflux, each 2h; Merge extractive liquid, is concentrated into density 1.08; Concentrated solution added in the 500ml water be dispersed into suspension, add the 500ml petroleum ether extraction 3 times, combining extraction liquid reclaims solvent to doing; Getting petroleum ether extraction part extractum, add and cross normal phase silicagel column after purification on normal-phase silica gel is mixed appearance, is that petroleum ether and the ethyl acetate solution of 50:1 is that eluant carries out eluting with the volume ratio, collects eluent, after concentrating, promptly gets.
9. the application of the Rhizoma Chuanxiong extract of claim 1-6 in the preparation antithrombotic reagent.
10. pharmaceutical composition is comprising Rhizoma Chuanxiong extract and pharmaceutically acceptable carrier or the excipient of claim 1-6.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980237A (en) * | 2014-05-22 | 2014-08-13 | 山西大学 | Method for separating and extracting ligustilide from radices levistici |
| CN109091516A (en) * | 2018-10-17 | 2018-12-28 | 四川省中医药科学院 | It is a kind of for antipyretic Chinese medicine composition |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1989984A (en) * | 2005-12-31 | 2007-07-04 | 天津天士力现代中药研究开发有限公司 | Chuanxiong rhizome effective ingredient, preparing method, preparation and use thereof |
| CN102631387A (en) * | 2012-04-24 | 2012-08-15 | 天津大学 | Preparation containing ligustilide type component for treating cardio-cerebrovascular disease and preparation method thereof |
| CN102824382A (en) * | 2012-08-23 | 2012-12-19 | 天津中医药大学 | Method for preparing Ligusticum wallichii lactone extract having anti-liquid-accumulation activity, and use |
-
2012
- 2012-10-12 CN CN201210301655.3A patent/CN102813687B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1989984A (en) * | 2005-12-31 | 2007-07-04 | 天津天士力现代中药研究开发有限公司 | Chuanxiong rhizome effective ingredient, preparing method, preparation and use thereof |
| CN102631387A (en) * | 2012-04-24 | 2012-08-15 | 天津大学 | Preparation containing ligustilide type component for treating cardio-cerebrovascular disease and preparation method thereof |
| CN102824382A (en) * | 2012-08-23 | 2012-12-19 | 天津中医药大学 | Method for preparing Ligusticum wallichii lactone extract having anti-liquid-accumulation activity, and use |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980237A (en) * | 2014-05-22 | 2014-08-13 | 山西大学 | Method for separating and extracting ligustilide from radices levistici |
| CN103980237B (en) * | 2014-05-22 | 2016-01-20 | 山西大学 | A kind of method of separation and Extraction Z-ligustilide from Root of Garden Lovage |
| CN109091516A (en) * | 2018-10-17 | 2018-12-28 | 四川省中医药科学院 | It is a kind of for antipyretic Chinese medicine composition |
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