CN1600755A - General flavones of hawthorn fruit, preparation method and application - Google Patents
General flavones of hawthorn fruit, preparation method and application Download PDFInfo
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- CN1600755A CN1600755A CN 03160027 CN03160027A CN1600755A CN 1600755 A CN1600755 A CN 1600755A CN 03160027 CN03160027 CN 03160027 CN 03160027 A CN03160027 A CN 03160027A CN 1600755 A CN1600755 A CN 1600755A
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- hawthorn fruit
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Abstract
The invention provides may bloom general flavone which can be expected for treating and preventing heart-head vascellum diseases, and the prepn, method. The may bloom general flavone and its preparation produced by the invention method can be used to treat and prevent coronary disease, stenocardia, myocardial infarction, hypertension, hyperlipemia, arythmia etc, and retrogressive pathologic changement of heart-head vascellum caused by said diseases.
Description
(1) technical field
The present invention relates to total flavones that a kind of plant amedica extracts and preparation method thereof and application, be specifically related to a kind of treatment and the hawthorn fruit total flavones of prevention diseases of cardiovascular and cerebrovascular systems and the preparation technology of preparation thereof.
(2) background technology
Hawthorn fruit is the mature fruit of rosaceous plant hawthorn Crataegus pinnatifida Bunge, Fruit of Pashi Pear Crataegus pinnatifidaBunge var.major N.E.Br..The Compendium of Material Medica record: hawthorn " sour sweet tepor; it is long-pending to help digestion; invigorating the spleen ", title hawthorn in modern age " Records of Tradition Chinese and Western Medicine in Combination " " be apt to into blood system the key medicine of stagnation resolvation; ... and be apt to into the gas branch to open obstruction of the circulation of vital energy phlegm knot; treat trusted subordinate's pain ... if help it with sweet medicine, stagnation resolvation blood and do not hinder new blood, open strongly fragrant gas and do not hinder healthy tendency, the outstanding peace of its property also." we find in the systematic study to hawthorn fruit; the hawthorn fruit total flavones has and reduces serum total cholesterol, triglyceride level; promote myocardial contraction; increase cardiac output and coronary flow, prevents and alleviates expeirmental myocardial ischemia anoxic and myocardial necrosis, dwindles myocardial infarct size; the protection cardiac muscle is not damaged; atherosclerosis, brings high blood pressure down, and improves effects such as hemorheology; The hawthorn fruit total flavones can also improve the susceptibility of cardiac muscle to the cardiotonic glycoside effect in addition, weakens myocardium irritability and conductivity, has effects such as anti-ventricular fibrillation, atrial fibrillation and paroxysmal irregular pulse.
(3) summary of the invention
The object of the present invention is to provide the preparation method and the application of the hawthorn fruit total flavones of a kind of treatment and prevention diseases of cardiovascular and cerebrovascular systems.
The hawthorn fruit total flavones of the present invention's treatment and prevention diseases of cardiovascular and cerebrovascular systems is to be raw material with the hawthorn fruit, be prepared from by solvent extraction, purifying, l-Epicatechol in the products obtained therefrom, Quercetin, Quercetin 3-galactoside, main component total contents such as vitexin rhamnoside and catechin polymkeric substance are greater than 50%.Step is as follows: after the hawthorn fruit chopping, use solvent extraction, can repeat to extract 1~3 time, extracting solution concentrates, depositing in water, and filtrate is made with extra care with solvent extraction and/or with silica gel, aluminum oxide, polymeric amide or macroporous resin column, refined products and depositing in water precipitation are merged, obtain the hawthorn fruit total flavones.
Extracting solvent can be methyl alcohol, ethanol, acetone, 30%~95% aqueous methanol, 30%~95% aqueous ethanol, 30%~95% aqueous acetone, vinyl acetic monomer or ritalin.
Extracting method can be backflow, dipping, diacolation, microwave extraction or supersound extraction.
Extracting process can be conventional organic solvent extraction or supercritical CO
2Extraction, the extraction organic solvent can be halohydrocarbon, vinyl acetic monomer, ritalin or propyl carbinol.
Silica gel and alumina column chromatography adopt the chloroform-methanol gradient elution, collect 10: 1~2: 1 wash-out parts of chloroform-methanol, and macroporous resin and polyamide column chromatography adopt water-ethanol or methyl alcohol gradient elution, collect 20%~80% ethanol or methanol-eluted fractions part.
The hawthorn fruit total flavones adds relevant pharmaceutical aids, can be made into various oral dosage forms and injection, comprise capsule, tablet, granule, mixture (oral liquid), pill, capsule and pill (soft capsule) agent, pellet, microcapsule, film coating tablet, sugar coated tablet, contain tablet, various oral sustained release, controlled release form and injection.
Hawthorn fruit total flavones and preparation thereof can be used as the medicine and the healthcare products of treatment and prevention diseases of cardiovascular and cerebrovascular systems, particularly be used for treatment and prevention coronary heart disease, stenocardia, myocardial infarction, vascular hypertension, hyperlipidaemia, disease such as irregular pulse and change by degeneration pathology such as the caused heart of above-mentioned illness, the cerebrovasculars.
Advantage of the present invention is: use hawthorn fruit total flavones and preparation thereof that the inventive method obtains, constant product quality is easily controlled, the active constituent content height, has remarkable reduction serum total cholesterol, triglyceride level, bring high blood pressure down, atherosclerosis, promote myocardial contraction, increase cardiac output and coronary flow, prevent and alleviate expeirmental myocardial ischemia to damage, anti-ventricular fibrillation, effects such as atrial fibrillation and paroxysmal irregular pulse, be used for the treatment of and prevent coronary heart disease, stenocardia, myocardial infarction, vascular hypertension, hyperlipidaemia, diseases such as irregular pulse and by the caused heart of above-mentioned illness, degeneration pathology such as the cerebrovascular change, and have good effect, the advantage that cost is low.
(4) description of drawings
Fig. 1 is the process flow sheet of embodiment 1.
Fig. 2 is the process flow sheet of embodiment 2.
Fig. 3 is that the hawthorn fruit total flavones is to the hypertensive table that influences of rat experiment.
Fig. 4 is the influence table of hawthorn fruit total flavones to experimental hyperlipidemia rabbit anteserum cholesterol and triglyceride level.
Fig. 5 is the influence table of hawthorn fruit total flavones to anesthetized dog coronary artery ligation myocardial ischemia ST section.
Fig. 6 causes the provide protection table of myocardial ischemia to rabbit injection Posterior Pituitary for the hawthorn fruit total flavones.
Fig. 7 is the influence table of hawthorn fruit total flavones to anesthesiaing dog heart blood flowing dynamics and coronary artery flow.
Fig. 8 is the effect table of rat ventricular due to the anti-napelline of hawthorn fruit total flavones.
Fig. 9 is a l-Epicatechol, Quercetin, Quercetin 3-galactoside, the structure iron of vitexin rhamnoside.
(5) embodiment
Embodiment 1: the preparation of hawthorn fruit total flavones
Hawthorn fruit is shredded, add one times of amount 95% alcohol immersion 2 days, and repeated to extract united extraction liquid 2 times, filter, filtrate decompression is concentrated into relative density 1.15~1.20, adds the water of 1 times of volume in concentrated solution, and the limit edged stirs, left standstill 12 hours, filter, and use the less water washing precipitation, the precipitation drying for standby.Filtrate is divided 4 extractions with 4 times of volumes of acetic acid ethyl esters, and 65 ℃ of concentrating under reduced pressure acetic acid ethyl acetate extracts are to cream, add drying precipitated, mixing, 65 ℃ are drying to obtain the hawthorn fruit total flavones.Process flow sheet is seen Fig. 1.
Embodiment 2: the preparation of hawthorn fruit total flavones
Hawthorn fruit is shredded, add one times of amount 95% alcohol immersion 2 days, and repeated to extract united extraction liquid 2 times, filter, filtrate decompression is concentrated into relative density 1.15~1.20, adds the water of 1 times of volume in concentrated solution, and the limit edged stirs, left standstill 12 hours, filter, and use the less water washing precipitation, the precipitation drying for standby.Macroporous resin column on the filtrate washes with water earlier and removes impurity, continuous uses 75% ethanol elution, collects 75% ethanol eluate, is evaporated to cream, add drying precipitated, mixing, 65 ℃ are drying to obtain the hawthorn fruit total flavones.Process flow sheet is seen Fig. 2.
Embodiment 3: the hawthorn fruit total flavones is to the hypertensive influence of rat experiment (acute renal artery stenotic type)
Get the healthy SD rat, ♂, 250-300g is divided into administration group and control group at random, and successive administration is 3 days after weighing, and control group is given physiological saline.Vetanarcol with 0.3% during experiment are anaesthetized 1ml/100g, prostrate being fixed in deducts chest, the small of the back hair on the rat operating table, cut skin to third lumbar vertebra along median line from the 10th thoracic vertebrae, 1.5-2cm and under the rib of left side apart from vertebra 1cm place, separate left kidney, with kidney the base of a fruit with little metal clip clamping 4-5 hour.Separate tracheae, insert trachea cannula, ligation.Separate carotid artery, the plastics tubing that will contain 0.1% heparin-saline inserts arteria carotis communis, and ligation is fixed.Another termination blood pressure transducer inserts four roads connection, recording blood pressure.Decontrol the little metal clip of kidney the base of a fruit, rat blood pressure is increased to plateau value, recording blood pressure gradually.Experimental result is seen accompanying drawing 3.
Annotate: hawthorn fruit total flavones and physiological saline are relatively
*P<0.05,
*P<0.01
Embodiment 4: the hawthorn fruit total flavones is to the influence of experimental hyperlipidemia rabbit anteserum cholesterol and triglyceride level
Select basal feed to stablize 2 all rabbit about body weight 2kg afterwards, be divided into 3 groups at random by body weight, every group when giving basal feed, irritate stomach once a day and give cholesterol 0.2g/kg (adding lard 2ml dissolves in), administration group and positive controls are respectively irritated stomach and give hawthorn fruit total flavones and zhibituo every days.Model group is given physiological saline.Carried out for 8 weeks continuously.3000rpm is centrifugal by ear edge vein exploitating blood respectively at 2 after the moulding, 4,6,8 weeks, and separation of serum is equipped with to be surveyed.Experimental result is seen accompanying drawing 4.
Annotate: hawthorn fruit total flavones and model group are relatively
*P<0.05,
*P<0.01,
* *P<0.001.
Embodiment 5: the hawthorn fruit total flavones is to the influence of anesthetized dog coronary artery ligation myocardial ischemia ST section
Get 20 of dogs, 8-12kg, ♀ ♂ half and half divides 4 groups at random, and 1ml/Kg is anaesthetized with 3% vetanarcol in the back of weighing, and lies on the back and is fixed on the operating table.Peel off tracheae and insert respirator, peel off muscle and expose heart, ligation dog left anterior descending coronary artery writes down one section electrocardiogram(ECG.Duodenal administration is after the record administration 30,45,13 the visceral pericardium electrocardiogram(ECG of 60min.Experimental result is seen accompanying drawing 5.
Annotate: compare before the administration of hawthorn fruit total flavones with after the administration
ΔP<0.05,
The Δ ΔP<0.01,
Δ Δ ΔP<0.01; Hawthorn fruit total flavones and physiological saline are relatively
*P<0.05,
*P<0.01,
* *P<0.001.
Embodiment 6: the hawthorn fruit total flavones causes the provide protection of myocardial ischemia to rabbit injection Posterior Pituitary
Get body weight and be 10 of the healthy rabbits of 1.5-2.0kg, the male and female dual-purpose, be divided into each 5 of control group and administration groups at random, the administration group is irritated stomach and give the hawthorn fruit total flavones every day, for three days on end, in administration in the 3rd day after one hour, clear-headed back of the body position is fixing, traces normal II lead electrocardiogram, by auricular vein injection Posterior Pituitary 4u/kg, 30s has annotated, and recording ecg changes.Experimental result is seen accompanying drawing 6.
Embodiment 7: the hawthorn fruit total flavones is to the influence of anesthesiaing dog heart blood flowing dynamics and coronary artery flow
Get 5 hybrid dogs about body weight 10kg, vetanarcol 30mg/kg anesthesia, the right side is faced upward the position and is fixed on the operating table, separate tracheae in order to artificial respiration, separate arteria carotis communis and survey arteriotony, the 4th ~ 5 intercostal is opened chest in the left side, expose heart, open respirator and carry out the malleation artificial respiration, vertically cut pericardium and separate aorta ascendens and ramus descendens anterior arteriae coronariae sinistrae top, measure cardiac output and coronary flow, left ventricle apex intubate is measured left ventricular pressure, write down the II lead electrocardiogram simultaneously to measure heart rate, above-mentioned every index synchronous recording on eight road physiographs.At first write down the preceding above-mentioned every index of administration, duodenum is given the hawthorn fruit total flavones then, the variation of every index after the record administration.Experimental result is seen accompanying drawing 7.
Annotate: compare after the administration of hawthorn fruit total flavones with before the administration
The Δ ΔP<0.01
* *P<0.001.
Embodiment 8: the effect of rat ventricular due to the anti-napelline of hawthorn fruit total flavones
Get 30 of 200g left and right sides SD rats, be divided into 3 groups at random, physiological saline group, Quinidine group, administration group are irritated stomach and are given the urethane intraperitoneal anesthesia after 1 hour of hawthorn fruit total flavones, record II lead electrocardiogram, per minute 0.8 μ g/200g constant speed is injected napelline solution, and the record generation chamber is (VP), chamber speed (VT), the consumption of napelline when (VF) quivered in the chamber early.Experimental result is seen accompanying drawing 8.
Annotate: hawthorn fruit total flavones group and physiological saline group are relatively
* *P<0.01.
Embodiment 9: the preparation of hawthorn fruit total flavone capsule agent
Prescription: (1000)
Hawthorn fruit total flavones 225g
Micropowder silica gel 25g (in add 24.5g/ add 0.5g)
Dehydrated alcohol Q.S
Preparation technology: the hawthorn fruit total flavones was pulverized 100 mesh sieves, take by weighing recipe quantity, with 98% of recipe quantity micropowder silica gel, cross 100 mesh sieves, mixing is with dehydrated alcohol system softwood, with 20 mesh sieve system particles, place 50 ℃ of loft drier forced air dryings 2 hours, take out dried particle, add remaining micropowder silica gel with the whole grain of 20 mesh sieves, mixing, the can capsule, check, packing.
Claims (8)
1. hawthorn fruit total flavones and preparation method thereof and application, it is characterized in that: be raw material with the hawthorn fruit, form by solvent extraction, depositing in water, extraction or chromatography are refining, gained total flavones main component is a l-Epicatechol, Quercetin, Quercetin 3-galactoside, vitexin rhamnoside and catechin polymkeric substance, its total content is greater than 50%.
2. according to the preparation method of the described hawthorn fruit total flavones of claim 1, it is characterized in that: extracting solvent can be methyl alcohol, ethanol, acetone, 30%~95% aqueous methanol, 30%~95% aqueous ethanol, 30%~95% aqueous acetone, vinyl acetic monomer or ritalin.
3. according to the preparation method of the described hawthorn fruit total flavones of claim 1, it is characterized in that: extracting method can be backflow, dipping, diacolation, microwave extraction or supersound extraction.
4. according to the preparation method of the described hawthorn fruit total flavones of claim 1, it is characterized in that: extracting process can be conventional organic solvent extraction or supercritical CO 2 extraction, and the extraction organic solvent can be halohydrocarbon, vinyl acetic monomer, ritalin or propyl carbinol.
5. according to the preparation method of the described hawthorn fruit total flavones of claim 1, it is characterized in that: chromatography method can be silica gel column chromatography, alumina column chromatography, polyamide column chromatography or macroporous resin column chromatography.
6. according to the application of the described hawthorn fruit total flavones of claim 1, it is characterized in that: can be as the application of preparation treatment and prevention diseases of cardiovascular and cerebrovascular systems medicine or healthcare products.
7. according to the application of the described hawthorn fruit total flavones of claim 5, it is characterized in that: can and prevent coronary heart disease, stenocardia, myocardial infarction, vascular hypertension, hyperlipidaemia as the preparation treatment, irregular pulse and the application that changes medicine by the caused heart of above-mentioned illness, cerebrovascular degeneration pathology.
8. according to the application of the described hawthorn fruit total flavones of claim 1, it is characterized in that: in total flavones, add relevant pharmaceutical aids, can be made into various oral dosage forms and injection, comprise capsule, tablet, granule, mixture (oral liquid), pill, capsule and pill (soft capsule) agent, pellet, microcapsule, film coating tablet, sugar coated tablet, contain tablet, various oral sustained release, controlled release form and injection.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101869581B (en) * | 2009-04-24 | 2012-07-11 | 湖北中烟工业有限责任公司 | Technical method for extracting active component from Chinese herbal medicine |
CN108117558A (en) * | 2016-11-28 | 2018-06-05 | 勐海茶业有限责任公司 | The method that Taide promise A and Taide promise B is split from fermented tea |
CN108117559A (en) * | 2016-11-28 | 2018-06-05 | 勐海茶业有限责任公司 | The method that the mixture of Taide promise A and Taide promise B is separated from fermented tea |
CN108645951A (en) * | 2018-05-14 | 2018-10-12 | 山东省中医药研究院 | A kind of thin-layer identification method of fructus crataegi medicinal material and medicine materical crude slice |
-
2003
- 2003-09-23 CN CN 03160027 patent/CN1600755A/en active Pending
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101869581B (en) * | 2009-04-24 | 2012-07-11 | 湖北中烟工业有限责任公司 | Technical method for extracting active component from Chinese herbal medicine |
CN108117558A (en) * | 2016-11-28 | 2018-06-05 | 勐海茶业有限责任公司 | The method that Taide promise A and Taide promise B is split from fermented tea |
CN108117559A (en) * | 2016-11-28 | 2018-06-05 | 勐海茶业有限责任公司 | The method that the mixture of Taide promise A and Taide promise B is separated from fermented tea |
CN108117559B (en) * | 2016-11-28 | 2020-07-31 | 勐海茶业有限责任公司 | Method for separating tedenox A and tedenox B mixture from fermented tea |
CN108117558B (en) * | 2016-11-28 | 2020-10-30 | 勐海茶业有限责任公司 | Method for separating teddenox A and teddenox B from fermented tea |
CN108645951A (en) * | 2018-05-14 | 2018-10-12 | 山东省中医药研究院 | A kind of thin-layer identification method of fructus crataegi medicinal material and medicine materical crude slice |
CN108645951B (en) * | 2018-05-14 | 2019-10-18 | 山东省中医药研究院 | A kind of thin-layer identification method of fructus crataegi medicinal material and medicine materical crude slice |
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