CN102145039A - Traditional Chinese medicine for treating cardiovascular diseases and preparation method thereof - Google Patents
Traditional Chinese medicine for treating cardiovascular diseases and preparation method thereof Download PDFInfo
- Publication number
- CN102145039A CN102145039A CN2010101067195A CN201010106719A CN102145039A CN 102145039 A CN102145039 A CN 102145039A CN 2010101067195 A CN2010101067195 A CN 2010101067195A CN 201010106719 A CN201010106719 A CN 201010106719A CN 102145039 A CN102145039 A CN 102145039A
- Authority
- CN
- China
- Prior art keywords
- ethanol
- water
- herba clinopodii
- filtrate
- concentrated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a traditional Chinese medicine with effects of activating blood circulation, eliminating blood stasis and treating cardiovascular diseases, and a preparation method of Clinopodium chinense total flavones in the traditional Chinese medicine. The effective ingredient of the traditional Chinese medicine is total flavones extracted from Clinopodium chinense or Clinopodium polycephalum. The preparation method of Clinopodium chinense total flavones mainly comprises extraction, enrichment and refinement. The traditional Chinese medicine provided by the invention can basically control the diseases, has small side effect, low incidence rate of adverse reactions and definite therapeutic effect, and can be administered for a long period of time.
Description
Technical field
The present invention relates to the field of Chinese medicines, specifically is Chinese medicine-Herba Clinopodii Polycephali total flavones of a kind of blood circulation promoting and blood stasis dispelling, treatment cardiovascular disease and preparation method thereof.
Background technology
Cardiovascular disease (CVD) is the disease general name that a big class influences heart and blood vessel, comprises coronary heart disease (CHD), cerebrovascular disease, hypertension and peripheral angiopathy (PVD); Also comprise other diseases such as rheumatic heart disease (because damage that rheumatic fever causes heart) and congenital heart disease (congenital cardiac structure is unusual).CVD and myocardial infarction, angina pectoris and apoplexy all are related.The accident that comprises myocardial infarction and apoplexy is mainly because atherosclerosis causes, and promptly fatty material (as cholesterol, platelet and cell debris) is in the chronic deposition of the arterial blood tube wall of supply heart and brain.Deposit forms local damage or atheromatous plaque.Pass in time, these local damages increase gradually and thicken, and cause blood vessels caliber to attenuate, and have reduced the blood flow by blood vessel.It is stiff that blood vessel also becomes, and elasticity reduces.
The cardiovascular diseases causes 1,750 ten thousand people's death every year.Have every year 7600000 people to die from heart disease, 5,700,000 people die from apoplexy.Expect the year two thousand twenty, the whole world will reach 2,500 ten thousand people because of the CVD death toll.Therefore, in necessarily global cardiovascular patient, especially cardiovascular disease high-risk patient,, reduce cardiovascular disease incidence rate and mortality rate, become a urgent day by day great public health problem how by effective intervention means for number.The whole world about 1/3 people dies from cardiovascular, its leapt to the first cause of the death of position.And show that according to current research the cardiovascular high-risk patient increases salvo newly, can pass through pharmaceutical intervention, effectively prevent death that cardiovascular causes, disable.Analysis expert, 80% coronary heart disease and cerebrovascular disease all cause owing to regulatable risk factor.Show according to statistics, cardiovascular and cerebrovascular disease sickness rate cumulative year after year, development are rapidly, also be to constitute one of China's population major causes of death, annual about 2,600,000 people die from cardiovascular and cerebrovascular disease, wherein angina pectoris, myocardial infarction, various arrhythmia, cardiovascular disease such as chronic congestive heart failure are occurred frequently, clinical with uncomfortable in chest, chest pain, cardiopalmus, feel suffocated, dyspnea etc. is primary symptom, motherland's medical science is examined and is the thoracic obstruction, angina pectoris, cardiopalmus, palpitation with a distress feeling, the syndrome of dyspnea etc.The Chinese medicine cardiovascular disease obtains curative effect preferably, and side effect is little, adverse reaction rate is low, can take by longer-term.
Beneficial effect of the present invention is with meaning: the Herba Clinopodii Polycephali total flavones be with the dry aerial parts of the Labiatae Clinopodium plant Clinopodium Polycephalum Herba Clinopodii (Herba Clinopodii Polycephali) (Clinopodiumpolycephalum) or Herba Clinopodii Polycephali (C.chinensis) extract, separate, refining obtaining.Wherein " Clinopodium Polycephalum Herba Clinopodii (Herba Clinopodii Polycephali) " beginning is stated from " Zhiwu Mingshi Tukao " (1848), mainly is distributed in ground such as Anhui, Hubei, Henan, Jiangxi, Guangxi, Guizhou, Yunnan, Sichuan, and all herbal medicine of using among the people has the effect of heat-clearing and toxic substances removing, cooling blood for hemostasis.The Herba Clinopodii Polycephali total flavones is one of main component of the Clinopodium Polycephalum Herba Clinopodii (Herba Clinopodii Polycephali) (Herba Clinopodii Polycephali), and we discover the active drug that can be used as preparation treatment cardiovascular disease, and simultaneously for further comprehensive utilization medical material, the development that drives mountain area economy has very high realistic meaning.
Summary of the invention
The invention provides the preparation method of Herba Clinopodii Polycephali total flavones in a kind of blood circulation promoting and blood stasis dispelling, the Chinese medicine for the treatment of cardiovascular disease and the Chinese medicine thereof, described Chinese medicine is control disease fundamentally, and side effect is little, adverse reaction rate is low, and determined curative effect, can take for a long time.
Pharmacodynamics test of the present invention:
1, experiment medicine: Herba Clinopodii Polycephali total flavones (CTF) reaches 53.5% (saponin reaction negative) in monarda glycoside content;
2, positive control medicine:
The FUFANG DANSHEN DIWAN specification: the 27mg/ ball, lot number: 20080303, Tianjin Tasly Pharmaceutical Co., Ltd produces
The Aspirin Enteric-coated Tablets specification: the 25mg/ sheet, lot number: 080506, Baijingyu Pharmaceutical Co., Ltd., Nanjing produces
3, experiment solvent: carboxymethylcellulose sodium solution (CMC-Na solution)
4, route of administration: irritate stomach
5, animal origin, kind
The healthy SD rat, body weight: 200-250g, male and female dual-purpose; Effluent south medical university provides credit number: SCXK (Henan) 2005-00001, cleaning level.Normally raised 3 days at laboratory before each treated animal experiment
6, experiment reagent:
Adrenalin hydrochloride injection: provide lot number by Shanghai Hefeng Pharmaceutical Co., Ltd.: 080104
Thrombin (Thr): provide by sigma company
Adenosine diphosphate (ADP) (ADP): provide by sigma company
PT test kit: provide lot number by Shanghai Rongsheng Bioisystech Co., Ltd: 20080507
APTT test kit: provide lot number by Shanghai Rongsheng Bioisystech Co., Ltd: 20080124
6-ketone-PG F
1 αRadioimmunity test kit: provide lot number by the Fu Rui of Beijing bio-engineering corporation: 20081026
TXB
2Radioimmunity test kit: provide lot number by the Fu Rui of Beijing bio-engineering corporation: 20081027
NO test kit: build up bio-engineering research by Nanjing lot number is provided: 20081102
7, experiment condition: room temperature 20-25 ℃, humidity 55-65%, air-conditioning control.
8, statistical method: test data is analyzed with the SPASS software statistics, and (x ± s) represent, result carry out the t check, and P＜0.05 has statistical significance for difference with mean ± standard deviation.
9, Herba Clinopodii Polycephali total flavones blood coagulation resisting function:
Compare with the blank group, each dosage group of Herba Clinopodii Polycephali total flavones all has the effect of prolong rats clotting time, and wherein high dose group and middle dosage group difference have statistical significance (P＜0.01), and low dose group difference also has statistical significance (P＜0.05).Experimental result shows that the Herba Clinopodii Polycephali total flavones has anticoagulant effect, has participated in intrinsic coagulation approach (seeing Table 1).
Table 1CTF to the influence of rat clotting time (CT) (x ± s, n=10)
*P＜0.05，**P＜0.01vs?control
Each dosage group of Herba Clinopodii Polycephali total flavones is energy significant prolongation rat activated partial thromboplastin time (P＜0.01, P＜0.05, vs control) all, and prothrombin time prolongs with the increasing of dosage, and wherein high, middle dosage can show
Work prolongs the PT time, and low dose group does not have obvious influence to the PT time.Experimental result shows that the Herba Clinopodii Polycephali total flavones acts on exogenous cruor pathway, has blood coagulation resisting function (table 2).
Table 2CTF to the influence of rat prothrombin time and activated partial thromboplastin time (x ± s, n=10)
*P＜0.05，**P＜0.01?vs?control
Each dosage group of Herba Clinopodii Polycephali total flavones can obviously shorten the rat euglobulin lysis time, and has significant differences (P＜0.01), each dosage group of Herba Clinopodii Polycephali total flavones also can shorten plasma clot dissolution time, with blank group comparing difference statistical significance (P＜0.01, P＜0.05, vs control) is arranged.Experimental result shows that the Herba Clinopodii Polycephali total flavones can improve the kinase whose activity level of fibrinolytic, thereby increases the activity (table 3) of fibrinolysin.
Table 3CTF to the influence of rat plasma EGCT and euglobulin lysis time (x ± s, n=10)
*P＜0.05，**P＜0.01?vs?control
Herba Clinopodii Polycephali total flavones high dose group and middle dosage group can significantly reduce the inductive platelet aggregation rate of ADP (P＜0.05), and the maximum suppression ratio of assembling is respectively 19.42%, 11.69%, though low dose can reduce platelet aggregation rate, effect is not remarkable.Show that the Herba Clinopodii Polycephali total flavones can effectively suppress the gathering (table 4) of the inductive rat platelet of ADP.
The table 4CTF to ADP induce platelet aggregation in the rat body influence (x ± s, n=10)
*P＜0.05，**P＜0.01?vs?control
Compare with the blank group, each dosage group of Herba Clinopodii Polycephali total flavones all makes thrombosis length obviously shorten, and high, middle dosage group has significant differences (P＜0.01), high dose group and middle dosage group wet weight of thrombus obviously alleviate (P＜0.01, P＜0.05), the thrombosis dry weight also has remarkable minimizing (P＜0.05), and Herba Clinopodii Polycephali total flavones low dose group weight in wet base and dry weight also have minimizing trend.Positive drug group thrombosis length, weight in wet base and dry weight all obviously reduce (P＜0.05).The result shows that the Herba Clinopodii Polycephali total flavones can effectively suppress the formation of rats in vitro thrombosis, and the high dose group effect is better than positive drug aspirin group and Composite Salvia Dropping Pill group (table 5).
Table 5 Herba Clinopodii Polycephali total flavones to the thrombotic influence of rats in vitro (x ± s, n=10)
*P＜0.05，**P＜0.01?vs?control
10, the Herba Clinopodii Polycephali total flavones influences stasis syndrome rat model hemorheological property:
Stasis syndrome model group rat whole blood viscosity, plasma viscosity, packed cell volume all generally increase, and comparing difference with the blank group has statistical significance (P＜0.01), show that the rat acute blood stasis model duplicates successfully.Each group of Herba Clinopodii Polycephali total flavones all can reduce whole blood contrast viscosity, plasma viscosity and the packed cell volume of stasis syndrome rat, compares difference with model group and has statistical significance (P＜0.01).The result shows, the high, medium and low three dosage groups of CTF all to blood stasis model sticking, dense, coagulate to change and obviously alleviate (table 6).
Table 6CTF to the influence of blood stasis rat blood rheological characteristic (x ± s, n=10)
*P＜0.05，**P＜0.01vs?control；
△P＜0.05，
△△P＜0.01?vs?Model
11, CTF is to blood stasis model rat plasma TXB
2, 6-keto-PGF
1 αContent and TXB
2/ 6-keto-PGF
1 αThe influence of ratio:
Compare model group TXB with the blank group
2Content has highly significant rising (P＜0.01), and 6-keto-PGF
1 αLevel presents highly significant reduction (P＜0.01), shows that the rat acute blood stasis model duplicates successfully.Herba Clinopodii Polycephali total flavones height, middle dosage group TXB
2Level all has significance to reduce (comparing P＜0.01 or P＜0.05 with model group), and Herba Clinopodii Polycephali total flavones high dose group 6-keto-PGF
1 αLevel presents ascendant trend, but in, low dose do not have statistical significance (with model group relatively, P＞0.05).The high, medium and low dosage group of Herba Clinopodii Polycephali total flavones TXB wherein
2/ 6-keto-PGF
1 αRatio descends obviously (comparing P＜0.01, P＜0.05 with the blank group).Aspirin group TXB
2Level has highly significant decline (comparing P＜0.01 with model group), TXB
2/ 6-keto-PGF
1 αRatio has obvious decline (comparing P＜0.05 with model group).Compound Salviae Miltiorrhizae group TXB
2Level all has significance to reduce (comparing P＜0.05 with model group), and 6-keto-PGF
1 αLevel significantly rises model group relatively, P＜0.05), TXB
2/ 6-keto-PGF
1 αRatio has highly significant decline (comparing P＜0.01 with model group).The result shows that the Herba Clinopodii Polycephali total flavones can obviously reduce TXB in the blood stasis rat plasma
2Content, high dose group is to 6-keto-PGF
1 αContent has certain rising effect, but a little less than the effect, Herba Clinopodii Polycephali total flavones low dose group is to TXB
2And 6-keto-PGF
1 αContent does not have obvious influence (P＞0.05) (table 7).
Table 7CTF is to blood stasis rat plasma TXB2,6-keto-PGF
1 αThe influence of content (x ± s, n=10)
*P＜0.05，**P＜0.01?vs?control；
△P＜0.05，
△△P＜0.01?vs?Model
Technical scheme of the present invention is:
The specific embodiment
The following embodiment of institute helps those skilled in the art to understand the present invention better, but does not limit the present invention in any way.
The active ingredient of the Chinese medicine of a kind of blood circulation promoting and blood stasis dispelling, treatment cardiovascular disease for or include the Herba Clinopodii Polycephali total flavones that from the Herba Clinopodii Polycephali or the Clinopodium Polycephalum Herba Clinopodii (Herba Clinopodii Polycephali), extracts.Chinese medicine is dosage forms such as capsule, granule, tablet, solution, pill, perhaps is injection type.
The preparation method of the Herba Clinopodii Polycephali total flavones in the Chinese medicine of blood circulation promoting and blood stasis dispelling, treatment cardiovascular disease.
Implementation method one:
(1), extract:
Extract the dry aerial parts of the Clinopodium Polycephalum Herba Clinopodii (Herba Clinopodii Polycephali) or Herba Clinopodii Polycephali, clean, cut into chunks, segment length 2-3cm, joining volume ratio then is soaked overnight, extraction, filtration in the water that 8-15 doubly measures, pH value is 6-7.5; It is 8-12 times of water extraction 1-2 time that medicinal residues after the filtration add volume ratio again, filters; Merging filtrate, the concentrated solution of relative density 1.10-1.30 is chilled to room temperature with concentrated solution when being evaporated to 60 ℃ of heat surveys, and adding ethanol to the weight that contains alcohol is 50-85%, stirs evenly, and leaves standstill 6-48 hour, filters filtrate recycling ethanol; Precipitation is with 50-85% washing with alcohol 1-2 time, each washing with alcohol weight be feed intake medical material weight 0.3-0.5 doubly, filter cleaning mixture, reclaim ethanol, and merge with filtrate,, relative density 1.15-1.20 when being concentrated into 60 ℃ of heat surveys then;
(2) enrichment:
The processing of upper prop liquid: the medicinal liquid after will concentrating, in crude drug weight: water volume ratio 3-0.5: 1 ratio adds neutral water, is heated to 30 ℃-50 ℃, stirs and makes dissolving, leaves standstill 2-24 hour, and A filters to get filtrate; Filter cake precipitation joins to stir in 0.1-0.2 by the medical material weight that feeds intake, the alkaline water liquid that pH value is 9-10 and makes dissolving, and B filters to get filtrate; Filtrate A and liquor B are merged, and precipitation is preserved;
Resin absorption: the filtrate after will merging is heated to 30-50 ℃, with D101 type, AB-8 type or D-201 type absorption with macroporous adsorbent resin, water or mass concentration are that the ethanol elution of 1-15% is closely colourless to eluent then, discard eluent, the reuse mass concentration is that the ethanol of 50-95% is washed till eluent and does not contain total saponins and flavone component;
The back eluent of resin absorption is merged, reclaim ethanol, relative density is the concentrated solution of 1.05-1.20 when being concentrated into 60 ℃ of heat surveys then, the water saturated n-butyl alcohol that adds the 1-5g/mL that is equivalent to medical material weight then in concentrated solution dissolves, heats, stirs evenly, move in the extractor, with the saturated 0.01-0.1mol/lNaOH solution washing of n-butyl alcohol to the alkali liquor layer to faint yellow-closely colourless, reuse n-butyl alcohol saturated aqueous solution washing 1-3 time; Merge alkali wash water and water lotion then, move in another extractor, add dilute hydrochloric acid while stirring and regulate pH value to 1-3, extremely faint yellow with water saturated n-butanol extraction to n-butanol layer, merge n-butanol extracting liquid, with n-butyl alcohol saturated aqueous solution washing 1-3 time, discarding water layer then, is 1 with n-butyl alcohol reclaim under reduced pressure to the volume ratio with the crude drug amount: 5-20;
(3) refining:
Add the 40-100 order silica gel of the 1-5% of the medical material weight that is equivalent to feed intake in the n-butyl alcohol concentrated solution after reclaim under reduced pressure, stir, dry, take out, grind well, adding volume ratio then is 6-8 ethanol extraction doubly 5-8 time, each 1 hour, filter, merge ethanol extract, then through decompression recycling ethanol, the residue extracting solution is concentrated near dried, drying under reduced pressure or spray drying, porphyrize, pulverize, sieve, packing gets the Herba Clinopodii Polycephali total flavones;
Ethanol extract after maybe will merging is chilled to room temperature, separates with polyamide column, collect ethanol extract, the reuse column volume is the 2-10BV ethanol elution, collects ethanol elution, and merge with ethanol extract, decompression recycling ethanol is concentrated near, drying under reduced pressure is done or spray drying, porphyrize is pulverized, and sieves, packing promptly gets the Herba Clinopodii Polycephali total flavones.
Implementation method two:
(1). extract:
Extract the dry aerial parts of the Clinopodium Polycephalum Herba Clinopodii (Herba Clinopodii Polycephali) or Herba Clinopodii Polycephali, clean, cut into chunks, segment length 2-3cm, joining volume ratio then is soaked overnight, extraction, filtration in the water that 8-15 doubly measures, pH value is 6-7.5; It is 8-12 times of water extraction 1-2 time that medicinal residues after the filtration add volume ratio again, filters; Merging filtrate, the concentrated solution of relative density 1.10-1.30 is chilled to room temperature with concentrated solution when being evaporated to 60 ℃ of heat surveys, and adding ethanol to the weight that contains alcohol is 50-85%, stirs evenly, and leaves standstill 6-48 hour, filters, and filtrate is with receipts ethanol; Precipitation is with 5-85% washing with alcohol 1-2 time, and each washing with alcohol weight is the 0.3-0.5 of medical material weight of feeding intake, filter cleaning mixture, reclaim ethanol, and merge with filtrate,, relative density 1.15-1.20 when being concentrated into 60 ℃ of heat surveys then;
(2). enrichment:
The processing of upper prop liquid: the medicinal liquid after will concentrating, in crude drug weight: water volume ratio 3-0.5: 1 ratio adds neutral water, is heated to 30 ℃-50 ℃, stirs and makes dissolving, leaves standstill 2-24 hour, and A filters to get filtrate; Filter cake precipitation joins to stir in 0.1-0.2 by the medical material weight that feeds intake, the alkaline water liquid that pH value is 9-10 and makes dissolving, and B filters to get filtrate; Filtrate A and liquor B are merged, and precipitation is preserved;
Resin absorption: the filtrate after will merging is heated to 30-50 ℃, with D101 type, AB-8 type or D-201 type absorption with macroporous adsorbent resin, water or mass concentration are that the ethanol elution of 1-15% is closely colourless to eluent then, discard eluent, the reuse mass concentration is that the ethanol of 50-95% is washed till eluent and does not contain total saponins and flavone component;
The back eluent of resin absorption is merged, reclaim ethanol, relative density is the concentrated solution of 1.05-1.20 when being concentrated into 60 ℃ of heat surveys then, the water saturated n-butyl alcohol that adds the 1-5g/mL that is equivalent to medical material weight then in concentrated solution dissolves, heats, stirs evenly, move in the extractor, with the saturated 0.01-0.1mol/lNaOH solution washing of n-butyl alcohol to the alkali liquor layer to faint yellow-closely colourless, reuse n-butyl alcohol saturated aqueous solution washing 1-3 time; Merge alkali wash water and water lotion then, move in another extractor, add dilute hydrochloric acid while stirring and regulate pH value to 1-3, extremely faint yellow with water saturated n-butanol extraction to n-butanol layer, merge n-butanol extracting liquid, with n-butyl alcohol saturated aqueous solution washing 1-3 time, discarding water layer then, is 1 with n-butyl alcohol reclaim under reduced pressure to the volume ratio with the crude drug amount: 5-20;
(3). refining:
Add the 40-100 order silica gel of the 1-5% of the medical material weight that is equivalent to feed intake in the n-butyl alcohol concentrated solution after reclaim under reduced pressure, stir, dry, take out, grind well, adding volume ratio then is 6-8 ethanol extraction doubly 5-8 time, each 1 hour, filter, merge ethanol extract, then through decompression recycling ethanol, the residue extracting solution is concentrated into to be done or spray drying, porphyrize is pulverized, and sieves, packing gets the Herba Clinopodii Polycephali total flavones; Ethanol extract after maybe will merging is chilled to room temperature, separates with polyamide column, collect ethanol extract, the reuse column volume is the 2-10BV ethanol elution, collects ethanol elution, and merge with ethanol extract, decompression recycling ethanol is concentrated near doing, decompression or spray drying, porphyrize is pulverized, and sieves, packing promptly gets the Herba Clinopodii Polycephali total flavones.
Claims (4)
1. the Chinese medicine of a blood circulation promoting and blood stasis dispelling, treatment cardiovascular disease is characterized in that: described effective components of Chinese medicinal for or include the Herba Clinopodii Polycephali total flavones that from Herba Clinopodii Polycephali, extracts.
2. the described Herba Clinopodii Polycephali total flavones that extracts from the Herba Clinopodii Polycephali or the Clinopodium Polycephalum Herba Clinopodii (Herba Clinopodii Polycephali) of claim 1 treats and/or prevents application in the cardiovascular disease medicine in preparation.
The Chinese medicine of blood circulation promoting and blood stasis dispelling according to claim 1, treatment cardiovascular disease, it is characterized in that: described Chinese medicine is capsule (soft capsule), granule (dry suspension), tablet (dispersible tablet), solution (syrup).
3. the preparation method one of the Herba Clinopodii Polycephali total flavones in the Chinese medicine of blood circulation promoting and blood stasis dispelling according to claim 1, treatment cardiovascular disease is characterized in that: may further comprise the steps:
(1). extract:
Get the dry aerial parts of the Clinopodium Polycephalum Herba Clinopodii (Herba Clinopodii Polycephali) or Herba Clinopodii Polycephali, clean, cutting, join soaked overnight, extraction, filtration in the water that pH value is 6-7.5; Medicinal residues after the filtration are extracting in water 1-3 time again, filters merging filtrate, then filtrate decompression being concentrated into 60 ℃ of heat survey relative densities is the concentrated solution of 1.10-1.30, concentrated solution is chilled to room temperature, adds ethanol and stir, left standstill 6-48 hour, filter, filtrate recycling ethanol, filter cake and precipitation washing with alcohol, filtration, cleaning mixture reclaims ethanol, then cleaning mixture and filtrate are merged, relative density is 1.15-1.20 when being concentrated into 60 ℃ of heat surveys;
(2). enrichment:
The processing of upper prop liquid: the medicinal liquid after will concentrating, in crude drug weight: water volume ratio is 0.5-3: 1 ratio adds neutral water, is heated to 30 ℃-50 ℃, stirs and makes dissolving, leaves standstill 2-24 hour, and A filters to get filtrate; The filter cake precipitation joins to stir in the alkaline water liquid that pH value is 9-10 and makes dissolving, and B filters to get filtrate; Filtrate A and liquor B are merged;
Resin absorption: the filtrate after will merging is heated to 30 ℃-50 ℃, with D101 type, AB-8 type or D-201 type absorption with macroporous adsorbent resin, then water or mass concentration be 1-15% to be eluted to eluent closely colourless, discarding eluent, is that the ethanol of 50-95% is washed till eluent and does not contain total saponins and flavone component with mass concentration then;
The back eluent of resin absorption is merged, reclaim ethanol, relative density is the concentrated solution of 1.05-1.20 when being concentrated into 60 ℃ of heat surveys then, adding water saturated n-butyl alcohol then in concentrated solution dissolves, heats, stirs evenly, move in the extractor, with the saturated 0.01-0.1mol/lNaOH solution washing of n-butyl alcohol to the alkali liquor layer to faint yellow-closely colourless, reuse n-butyl alcohol saturated aqueous solution washing 1-3 time; Merge alkali wash water and water lotion then, move in another extractor, add dilute hydrochloric acid while stirring and regulate pH value to 1-3, extremely faint yellow with water saturated n-butanol extraction to n-butanol layer, merge n-butanol extracting liquid, with n-butyl alcohol saturated aqueous solution washing 1-3 time, discarding water layer then, is 1 with n-butyl alcohol reclaim under reduced pressure to the volume ratio with the crude drug amount: 5-20;
(3). refining:
Add 40-100 purpose silica gel in the n-butyl alcohol concentrated solution after reclaim under reduced pressure, stirring, oven dry, taking-up grind well, and use ethanol extraction 5-8 time then, filter, merge ethanol extract, through decompression recycling ethanol, be concentrated into and do or spray drying porphyrize then, pulverize, sieve, packing promptly gets the Herba Clinopodii Polycephali total flavones; Ethanol extract after maybe will merging is chilled to room temperature, separates with polyamide column, collect ethanol extract, the reuse column volume is the 2-10BV ethanol elution, collects ethanol elution, and merge with ethanol extract, decompression recycling ethanol is concentrated into and does or spray drying porphyrize, pulverize, sieve, packing promptly gets the Herba Clinopodii Polycephali total flavones.
4. according to the preparation method two of the Herba Clinopodii Polycephali total flavones in the Chinese medicine of claim 1 blood circulation promoting and blood stasis dispelling, treatment cardiovascular disease, it is characterized in that: specifically may further comprise the steps:
Specifically may further comprise the steps:
(1). extract:
Extract the dry aerial parts of the Clinopodium Polycephalum Herba Clinopodii (Herba Clinopodii Polycephali) or Herba Clinopodii Polycephali, clean, cut into chunks, segment length 2-3cm, joining volume ratio then is soaked overnight, extraction, filtration in the water that 8-15 doubly measures, pH value is 6-7.5; It is 8-12 times of water extraction 1-2 time that medicinal residues after the filtration add volume ratio again, filters; Merging filtrate, the concentrated solution of relative density 1.10-1.30 is chilled to room temperature with concentrated solution when being evaporated to 60 ℃ of heat surveys, and adding ethanol to the weight that contains alcohol is 50-85%, stirs evenly, and leaves standstill 6-48 hour, filters filtrate recycling ethanol; Precipitation is with 5-85% washing with alcohol 1-2 time, and each washing with alcohol weight is the 0.3-0.5 of medical material weight of feeding intake, filter cleaning mixture, reclaim ethanol, and merge with filtrate,, relative density 1.15-1.20 when being concentrated into 60 ℃ of heat surveys then;
(2). enrichment:
The processing of upper prop liquid: the medicinal liquid after will concentrating, in crude drug weight: water volume ratio 3-0.5: 1 ratio adds neutral water, is heated to 30 ℃-50 ℃, stirs and makes dissolving, leaves standstill 2-24 hour, and A filters to get filtrate; Filter cake precipitation joins to stir in 0.1-0.2 by the medical material weight that feeds intake, the alkaline water liquid that pH value is 9-10 and makes dissolving, and B filters to get filtrate; Filtrate A and liquor B are merged, and precipitation is preserved;
Resin absorption: the filtrate after will merging is heated to 30-50 ℃, with D101 type, AB-8 type or D-201 type absorption with macroporous adsorbent resin, water or mass concentration are that the ethanol elution of 1-15% is closely colourless to eluent then, discard eluent, the reuse mass concentration is that the ethanol of 50-95% is washed till eluent and does not contain total saponins and flavone component;
The back eluent of resin absorption is merged, reclaim ethanol, relative density is the concentrated solution of 1.05-1.20 when being concentrated into 60 ℃ of heat surveys then, the water saturated n-butyl alcohol that adds the 1-5g/mL that is equivalent to medical material weight then in concentrated solution dissolves, heats, stirs evenly, move in the extractor, with the saturated 0.01-0.1mol/lNaOH solution washing of n-butyl alcohol to the alkali liquor layer to faint yellow-closely colourless, reuse n-butyl alcohol saturated aqueous solution washing 1-3 time; Merge alkali wash water and water lotion then, move in another extractor, add dilute hydrochloric acid while stirring and regulate pH value to 1-3, extremely faint yellow with water saturated n-butanol extraction to n-butanol layer, merge n-butanol extracting liquid, with n-butyl alcohol saturated aqueous solution washing 1-3 time, discarding water layer then, is 1 with n-butyl alcohol reclaim under reduced pressure to the volume ratio with the crude drug amount: 5-20;
(3). refining:
Add the 40-100 order silica gel of the 1-5% of the medical material weight that is equivalent to feed intake in the n-butyl alcohol concentrated solution after reclaim under reduced pressure, stir, dry, take out, grind well, adding volume ratio then is 6-8 ethanol extraction doubly 5-8 time, each 1 hour, filter, merge ethanol extract, then through decompression recycling ethanol, the residue extracting solution is concentrated into to be done or spray drying, porphyrize is pulverized, and sieves, packing gets the Herba Clinopodii Polycephali total flavones;
Ethanol extract after maybe will merging is chilled to room temperature, separates with polyamide column, collect ethanol extract, the reuse column volume is the 2-10BV ethanol elution, collects ethanol elution, and merge with ethanol extract, decompression recycling ethanol is concentrated near doing, decompression or spray drying, porphyrize is pulverized, and sieves, packing promptly gets the Herba Clinopodii Polycephali total flavones.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101067195A CN102145039A (en) | 2010-02-08 | 2010-02-08 | Traditional Chinese medicine for treating cardiovascular diseases and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101067195A CN102145039A (en) | 2010-02-08 | 2010-02-08 | Traditional Chinese medicine for treating cardiovascular diseases and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102145039A true CN102145039A (en) | 2011-08-10 |
Family
ID=44419641
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010101067195A Pending CN102145039A (en) | 2010-02-08 | 2010-02-08 | Traditional Chinese medicine for treating cardiovascular diseases and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102145039A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103664859A (en) * | 2012-09-05 | 2014-03-26 | 中国医学科学院药用植物研究所 | Novel isopentenyl naphthoquinone obtained in active fraction for promoting blood circulation to remove blood stasis in clinopodium chinense (Benth.) O. Kuntze. and preparation method thereof |
| CN104706720A (en) * | 2015-02-13 | 2015-06-17 | 新昌县大成生物科技有限公司 | Clinopodium chinense extract and application thereof in medicament for treating urinary calculus |
| CN106279318A (en) * | 2015-05-29 | 2017-01-04 | 中国医学科学院药用植物研究所 | The separation method of flavone compound and flavone composition in Herba Clinopodii Polycephali |
| CN108126006A (en) * | 2016-12-01 | 2018-06-08 | 林凡友 | The preparation process of clinopodium polycephalum oral preparation |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1891255A (en) * | 2005-06-09 | 2007-01-10 | 山东绿叶天然药物研究开发有限公司 | Blood total flavone extract, and its preparing method and use |
| CN101234159A (en) * | 2007-01-29 | 2008-08-06 | 陈晓坚 | Pharmaceutical combination with synergistic reaction |
-
2010
- 2010-02-08 CN CN2010101067195A patent/CN102145039A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1891255A (en) * | 2005-06-09 | 2007-01-10 | 山东绿叶天然药物研究开发有限公司 | Blood total flavone extract, and its preparing method and use |
| CN101234159A (en) * | 2007-01-29 | 2008-08-06 | 陈晓坚 | Pharmaceutical combination with synergistic reaction |
Non-Patent Citations (2)
| Title |
|---|
| 李国贤: "荫风轮总黄酮对心血管系统的作用", 《安徽大学学报(自然科学版)》 * |
| 迟海东等: "风轮菜属药用植物研究进展", 《沈阳药科大学学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103664859A (en) * | 2012-09-05 | 2014-03-26 | 中国医学科学院药用植物研究所 | Novel isopentenyl naphthoquinone obtained in active fraction for promoting blood circulation to remove blood stasis in clinopodium chinense (Benth.) O. Kuntze. and preparation method thereof |
| CN104706720A (en) * | 2015-02-13 | 2015-06-17 | 新昌县大成生物科技有限公司 | Clinopodium chinense extract and application thereof in medicament for treating urinary calculus |
| CN106279318A (en) * | 2015-05-29 | 2017-01-04 | 中国医学科学院药用植物研究所 | The separation method of flavone compound and flavone composition in Herba Clinopodii Polycephali |
| CN106279318B (en) * | 2015-05-29 | 2019-05-03 | 中国医学科学院药用植物研究所 | The separation method and flavone composition of flavone compound in calamint |
| CN108126006A (en) * | 2016-12-01 | 2018-06-08 | 林凡友 | The preparation process of clinopodium polycephalum oral preparation |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102145039A (en) | Traditional Chinese medicine for treating cardiovascular diseases and preparation method thereof | |
| CN102861123A (en) | Traditional Chinese medicine extract with effect on promoting angiogenesis as well as preparation method and application thereof | |
| CN101757391B (en) | Medicine composition for treating cardio-cerebral-vascular diseases and preparation method and application thereof | |
| CN107929544A (en) | The preparation method and applications of militarine positions and monomer in bletilla platymiscium | |
| CN101697989B (en) | Application of notoginseng and extract thereof in preparing medicaments for treating and/or preventing coronary artherosclerosis | |
| CN105056238A (en) | Medicine composition with anti-tumor activity, as well as preparation method and application thereof | |
| CN102028834B (en) | Compound Longxueji preparation and preparation method thereof | |
| CN104547026B (en) | Preparation method and application of salvia miltiorrhiza leave pseudo-ginseng extract | |
| CN101716253B (en) | Chinese medicinal preparation containing panax notoginseng, and preparation method thereof | |
| CN101380356B (en) | Tibetan medicine Duyiwei total flavone extract and extraction method and use thereof | |
| CN100506219C (en) | Notoginseng hemostatic and its preparing method | |
| CN103156870B (en) | Pharmaceutical composition of a kind of Cardiovarscular and preparation method thereof | |
| CN104547027B (en) | Preparation method and application of salvia miltiorrhiza leave and panax notoginseng leaf extract | |
| CN103263581A (en) | Shuangshen capsule for reducing blood sugar | |
| CN103800736A (en) | Pharmaceutical composition for treating hypertensive nephrosclerosis and application of pharmaceutical composition | |
| CN101926848B (en) | Medicinal composition for treating heart cerebrovascular diseases and preparation thereof | |
| CN108126116A (en) | A kind of preparation process of full rhizoma gastrodiae tablet | |
| CN101028311A (en) | Use of selaginella tamariscina | |
| CN104547025B (en) | Salvia miltiorrhiza and pseudo-ginseng leaf extract and preparation method thereof | |
| CN101549050B (en) | Traditional Chinese medicine composition for treating cardiovascular and cerebrovascular diseases and preparation method thereof | |
| CN101607070A (en) | A kind of pharmaceutical composition that is used for the treatment of cardiovascular and cerebrovascular disease | |
| CN112773839A (en) | Preparation method of improved sanhua soup | |
| CN1915266A (en) | Medicinal composition, preparation method and quality control method | |
| CN1915272A (en) | Medicinal composition, preparation method and quality control method | |
| CN1981819A (en) | Tree-peony root bark component, its preparation, making method and use |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20110810 |