CN101164546B - Vein-relaxing pain-relieving medicinal composition and preparation method and use thereof - Google Patents
Vein-relaxing pain-relieving medicinal composition and preparation method and use thereof Download PDFInfo
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- CN101164546B CN101164546B CN2006100969754A CN200610096975A CN101164546B CN 101164546 B CN101164546 B CN 101164546B CN 2006100969754 A CN2006100969754 A CN 2006100969754A CN 200610096975 A CN200610096975 A CN 200610096975A CN 101164546 B CN101164546 B CN 101164546B
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Abstract
The present invention relates to a medicine composition with the functions of promoting blood circulation, removing stasis, removing obstruction in the channels to relieve pain for effectively curing coronary heart disease and angina pectoris. It is made up by using (by wt%) 10-80% of bilobalide, 10-80% of breviscapine and 10-80% of ligustrazine hydrochloride as main effective components. Said invention also provides its preparation method and application.
Description
Technical field
The present invention relates to a kind of pharmaceutical composition, particularly a kind of vein-relaxing pain-relieving medicinal composition; The invention still further relates to the Preparation method and use of said composition.
Background technology
Coronary heart disease is the abbreviation of coronary heart disease, be a kind of because coronary artery stationarity (atherosclerosis) or dynamic property (vasospasm) stenosis or occlusion, the coronary circulation obstacle takes place, cause that myocardial oxygen is unbalance and cause myocardial ischemia-anoxemia or downright bad a kind of heart disease between needing, also be called ischemic heart desease.This sick basic lesion is angina pectoris, arrhythmia, heart failure, may die suddenly.
In recent decades, China progresses into senescence society, and this sick sickness rate presents more and more high trend in China, and owing to this sick sickness rate height, the fatality rate height of disabling, the healthy of the mankind in serious harm, and this sick diagnosis and treatment work more and more is subject to people's attention.Modern medicine treatment coronary heart disease generally adopts Drug therapy, operative treatment.Drug therapy can reduce anginal outbreak and myocardial infarction, the incidence rate of sudden cardiac death on the one hand; Can slow down the development of coronary heart disease on the other hand or its aspect of becoming better is changed.For example: use medicine, fat-reducing medicament, the anti-platelet activity medicine of control hypertension and diabetes and improve the coronary blood supply medicine and thrombolytic drug, antiarrhythmic drug or the like.Modern pharmacological research and Chinese medical theory facts have proved that part has the Chinese medicine material of strong blood circulation invigorating efficacies, can obviously improve the coronary blood supply situation, slow down the development of coronary heart disease, and its determined curative effect, safety non-toxic are subjected to numerous doctors patient's welcome and high praise deeply.
Summary of the invention
Technical problem to be solved by this invention is at the deficiencies in the prior art, and a kind of new, simple, compatibility a kind of vein-relaxing pain-relieving medicinal composition reasonable, evident in efficacy of prescription is provided.
Another technical problem to be solved by this invention has provided the preparation method of aforementioned pharmaceutical compositions.
Another technical problem to be solved by this invention has provided the medical usage of aforementioned pharmaceutical compositions.
Technical problem to be solved by this invention is to realize by following technical scheme.The present invention is a kind of vein-relaxing pain-relieving medicinal composition, is characterized in, the weight proportion of raw material consists of,
Bilobalide 10～80;
Breviscapine 10～80;
Ligustrazine hydrochloride 10～80.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described a kind of vein-relaxing pain-relieving medicinal composition is characterized in that the weight proportion of raw material consists of,
Bilobalide 20～60;
Breviscapine 20～60;
Ligustrazine hydrochloride 20～60.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described a kind of vein-relaxing pain-relieving medicinal composition is characterized in that the weight proportion of raw material consists of,
Bilobalide 30～40;
Breviscapine 30～40;
Ligustrazine hydrochloride 30～40.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described a kind of vein-relaxing pain-relieving medicinal composition is characterized in that the weight proportion of raw material consists of,
Bilobalide 40;
Breviscapine 30;
Ligustrazine hydrochloride 30.
Technical problem to be solved by this invention can also further realize by following technical scheme.The present invention is a kind of preparation method of vein-relaxing pain-relieving medicinal composition, is characterized in,
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 6-12 times of water gagings and decocts 2-3 times, each 1-3 hours, merge decocting liquid, and put and be chilled to room temperature, added suitable adsorbent stirring and adsorbing 12-48 hours, leave standstill filtration, collect adsorbent.Adsorbent adds 6-10 times of amounts of 50-95% ethanol backflow eluting, each 1-3 hours, filter, eluent merges, and is evaporated to 0.5-2g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 60-95% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 60-95% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 60-95% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 6-12 times of amounts of 75-95% ethanol lixiviate 2-3 time, each 1-3 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1-2g medical material/ml with hot water, add hydrochloric acid and regulate pH to 1-3, cold preservation 12-36 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 60-80% ethanol recrystallization repeatedly with water washing;
(3) get bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, make the medicine that to accept dosage form on any pharmaceutics.
The raw material bilobalide and the breviscapine of pharmaceutical composition of the present invention can adopt the inventive method to make, and also can adopt in the prior art disclosed method or conventional method to make, or directly select the commercially available prod for use; Ligustrazine hydrochloride of the present invention is recorded known substance by in 452 pages of the Chinese Pharmacopoeias in 1977, has clear and definite quality standard and list marketing, can adopt in the prior art disclosed method or conventional method to make, or directly select the commercially available prod for use.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described a kind of collateral dredging preparation of drug combination method of only uniting is characterized in,
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 9 times of water gagings and decocts 2 times, each 2 hours, merge decocting liquid, and put and be chilled to room temperature, add active carbon or chromatographic silica gel and made the adsorbent stirring and adsorbing 24 hours, leave standstill filtration, collect adsorbent; Adsorbent adds 8 times of 70% ethanol amount backflow eluting, each 2 hours, filter, eluent merges, and is evaporated to 1g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 80% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 80% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 80% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 9 times of amounts of 85% ethanol lixiviate 2 times, each 2 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1.5g medical material/ml with hot water, add hydrochloric acid and regulate pH to 2, cold preservation 24 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 70% ethanol recrystallization repeatedly with water washing;
(3) get bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, make injection.
A kind of vein-relaxing pain-relieving medicinal composition of the present invention can be used for preparing the treatment treating coronary heart disease and angina pectoris.
Be the drug efficacy study experiment that vein-relaxing pain-relieving medicinal composition of the present invention that the inventor did resists myocardial ischemia below.
Compositions is mixed with the medicinal liquid of variable concentrations with 0.9% sodium chloride injection.
1, coronary ligation is brought out the influence of rat acute myocardial infarction model
Rat is divided into 7 groups at random, and 12 every group, i.e. (1) sham operated rats: a silk thread is worn at the coronary artery place, refuses ligation, tail vein injection 0.9% sodium chloride injection 10ml/kg; (2) model group: ligation coronary artery, tail vein injection 0.9% sodium chloride injection 10ml/kg; (3) diltiazem group: ligation coronary artery, tail vein injection diltiazem injection 0.9mg/kg; (4) ligustrazine hydrochloride group: ligation coronary artery, tail vein injection ligustrazine hydrochloride 7.2mg/kg; (5) the high, medium and low dosage group of compositions: the ligation coronary artery, respectively at tail vein injection compositions 21.6,10.8,5.4mg/kg.0.5h behind the ligation coronary artery, tail vein injection 0.9% sodium chloride injection or medicinal liquid.After the ligation 5 hours, common carotid artery is got blood, and the separation of serum sample detects creatine kinase (CK), lactic acid dehydrogenase (LDH), malonaldehyde (MDA), superoxide dismutase (SOD).Take out heart rapidly and measure myocardial infarction area (IS), the infarct size percentage rate=myocardial infarction area area/myocardium gross area * % after getting blood.
The result: compositions and positive drug can make CK, LDH behind the myocardial ischemia, MDA and IS significantly reduce (P＜0.05), improve the content (P＜0.05) of SOD, table 1.
Table 1 compositions is brought out influence (n=10, the x ± SD) of rat acute myocardial infarction model to coronary ligation
Annotate: compare with the blank group,
△P＜0.05,
△ △P＜001; Compare with model
*P＜0.05,
*P＜0.01
2, pituitrin is brought out the influence that the Acute Myocardial Ischemia in Rats electrocardiogram changes
84 of the qualified rats of screening electrocardiogram, be divided into 7 groups at random, every group 12, be blank group and model group (iv0.9% sodium chloride injection 10ml/kg), diltiazem group (iv diltiazem injection 0.9mg/kg), ligustrazine hydrochloride group (iv ligustrazine hydrochloride 7.2mg/kg), the combination object height, in, low dose group (difference iv compositions 21.6,10.8,5.4mg/kg), after each organizes administration 5min, with pentobarbital sodium (30mg/kg, ip) anesthesia, the II of record 1min leads electrocardiogram, sublingual vein injection of pituitrin 1.2U/kg then, volume is 1ml/kg, annotated blank group sublingual vein injection isometric(al) 0.9% sodium chloride injection in 5～10s.Trace the electrocardiogram of instant, 15s, 30s, 1min, 2min, 5min.
The result: quiet notes pituitrin can bring out rat electrocardiogram generation significant change, compositions and positive drug can obviously be alleviated the change of the caused electrocardiogram J point of pituitrin, PR interval and PP interval, the prompting compositions can be alleviated myocardial ischemia due to the coronary spasm, sees Table 2.
Table 2 compositions is brought out the influence that the Acute Myocardial Ischemia in Rats electrocardiogram changes to pituitrin
J point variation (mv) (n=12, x ± SD)
Annotate: compare with the blank group,
△P＜0.05,
△ △P＜0.01; Compare with model
*P＜005,
*P＜001
The PR interval, change (ms) (n=12, x ± SD)
Annotate: compare with the blank group,
△P＜0.05,
△ △P＜0.01; Compare with model
*P＜005,
*P＜0.01
The PP interval, change (ms) (n=12, x ± SD)
Annotate: compare with the blank group,
△P＜0.05,
△ △P＜0.01; Compare with model
*P＜0.05,
*P＜001
3, compositions is to the influence of anoxia enduring time-to-live of mice normal pressure
Get 120 of mices, be divided into 6 groups, every group 20, be blank group and model group (iv0.9% sodium chloride injection 10ml/kg), diltiazem group (iv diltiazem injection 1.95mg/kg), ligustrazine hydrochloride group (iv ligustrazine hydrochloride 10.4mg/kg), the combination object height, in, low dose group (difference iv compositions 31.2,15.6,7.8mg/kg), after the administration 0.5 hour, put into the 250mL port grinding bottle (1 every bottle) that fills the 5g sodica calx respectively, seal bottleneck with vaseline, cover completely, make it air tight, timing immediately is an index with the respiratory arrest, observes mice because of the dead time of anoxia.Record mice hypoxia endurance time.
Result: compare with the blank group, but compositions and the time-to-live of diltiazem significant prolongation mice under the normobaric hypoxia situation see Table 3
Table 3 compositions is to the influence of anoxia enduring time-to-live of mice normal pressure (n=20, x ± SD)
Compare with blank,
*P＜0.05,
*P＜0.01
The present composition has blood circulation promoting and blood stasis dispelling, the removing obstruction in the collateral to relieve pain effect, and its prescription is simple, compatibility is reasonable, therapeutic effect is remarkable, can be used for treating the treatment of angina pectoris.The inventive method can extract bilobalide and breviscapine effectively by requirement of the present invention, and extract obtained middle impurity content is few, the yield height.
The specific embodiment
Embodiment 1.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 10;
Breviscapine 10;
Ligustrazine hydrochloride 80.
Its preparation method is, selects commercially available bilobalide, breviscapine and ligustrazine hydrochloride for use, adds pharmaceutic adjuvant, and technology is made tablet routinely, is used for the treatment of angina pectoris.
Embodiment 2.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 80;
Breviscapine 80;
Ligustrazine hydrochloride 10.
Its preparation method is, selects commercially available bilobalide, breviscapine and ligustrazine hydrochloride for use, adds pharmaceutic adjuvant, and technology is made granule routinely, is used for the treatment of angina pectoris.
Embodiment 3.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 10;
Breviscapine 10;
Ligustrazine hydrochloride 10.
Its preparation method is, selects commercially available bilobalide, breviscapine and ligustrazine hydrochloride for use, adds pharmaceutic adjuvant, and technology is made capsule routinely, is used for the treatment of angina pectoris.
Embodiment 4.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 10;
Breviscapine 80;
Ligustrazine hydrochloride 80.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made tablet routinely, is used for the treatment of angina pectoris.
Embodiment 5.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 80;
Breviscapine 10;
Ligustrazine hydrochloride 80.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made granule routinely, is used for the treatment of angina pectoris.
Embodiment 6.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 80;
Breviscapine 80;
Ligustrazine hydrochloride 80.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made capsule routinely, is used for the treatment of angina pectoris.
Embodiment 7.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 80;
Breviscapine 10;
Ligustrazine hydrochloride 10.
Its preparation method is,
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 6 times of water gagings and decocts 2 times, each 1 hour, merge decocting liquid, and put and be chilled to room temperature, added suitable adsorbent stirring and adsorbing 12 hours, leave standstill filtration, collect adsorbent.Adsorbent adds 6 times of 50% ethanol amount backflow eluting, each 1 hour, filter, eluent merges, and is evaporated to 0.5g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 60% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 60% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 60% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 6 times of amounts of 75% ethanol lixiviate 2 times, each 3 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1g medical material/ml with hot water, add hydrochloric acid and regulate PH to 1, cold preservation 12 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 60% ethanol recrystallization repeatedly with water washing;
(3) get silver-colored bilobalide, breviscapine and commercially available ligustrazine hydrochloride, add pharmaceutic adjuvant, make tablet, be used for the treatment of angina pectoris.
Embodiment 8.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 10;
Breviscapine 80;
Ligustrazine hydrochloride 10.
Its preparation method is,
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 12 times of water gagings and decocts 3 times, each 3 hours, merge decocting liquid, and put and be chilled to room temperature, added suitable adsorbent stirring and adsorbing 48 hours, leave standstill filtration, collect adsorbent.Adsorbent adds 10 times of 95% ethanol amount backflow eluting, each 3 hours, filter, eluent merges, and is evaporated to 2g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 95% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 95% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 95% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 12 times of amounts of 95% ethanol lixiviate 3 times, each 3 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 2g medical material/ml with hot water, add hydrochloric acid and regulate PH to 3, cold preservation 36 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 80% ethanol recrystallization repeatedly with water washing;
(3) get bilobalide, breviscapine and commercially available ligustrazine hydrochloride, add pharmaceutic adjuvant, make capsule, be used for the treatment of angina pectoris.
Embodiment 9.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 15;
Breviscapine 70;
Ligustrazine hydrochloride 70.
Its preparation method is,
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 7 times of water gagings and decocts 2 times, each 2 hours, merge decocting liquid, and put and be chilled to room temperature, added suitable adsorbent stirring and adsorbing 24 hours, leave standstill filtration, collect adsorbent.Adsorbent adds 7 times of 60% ethanol amount backflow eluting, each 2 hours, filter, eluent merges, and is evaporated to 1.5g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 70% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 70% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 70% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 8 times of amounts of 85% ethanol lixiviate 2 times, each 2 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1.5g medical material/ml with hot water, add hydrochloric acid and regulate PH to 2, cold preservation 24 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 70% ethanol recrystallization repeatedly with water washing;
(3) get bilobalide, breviscapine and the ligustrazine hydrochloride that extracts of technology routinely, add pharmaceutic adjuvant, make drop pill, be used for the treatment of angina pectoris.
Embodiment 10.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 70;
Breviscapine 15;
Ligustrazine hydrochloride 15.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made pill routinely, is used for the treatment of angina pectoris.
Embodiment 11.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 15;
Breviscapine 70;
Ligustrazine hydrochloride 15.
Its preparation method is, by art methods extract bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made injectable powder routinely, is used for the treatment of angina pectoris.
Embodiment 12.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 15;
Breviscapine 15;
Ligustrazine hydrochloride 70.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made infusion solution routinely, is used for the treatment of angina pectoris.
Embodiment 13.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 15;
Breviscapine 15;
Ligustrazine hydrochloride 15.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made capsule routinely, is used for the treatment of angina pectoris.
Embodiment 14.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 70;
Breviscapine 15;
Ligustrazine hydrochloride 70.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made tablet routinely, is used for the treatment of angina pectoris.
Embodiment 15.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 70;
Breviscapine 70;
Ligustrazine hydrochloride 70.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made drop pill routinely, is used for the treatment of angina pectoris.
Embodiment 16.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 60;
Breviscapine 20;
Ligustrazine hydrochloride 20.
Its preparation method is,
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 10 times of water gagings and decocts 3 times, each 2 hours, merge decocting liquid, and put and be chilled to room temperature, added suitable adsorbent stirring and adsorbing 36 hours, leave standstill filtration, collect adsorbent.Adsorbent adds 8 times of 70% ethanol amount backflow eluting, each 2 hours, filter, eluent merges, and is evaporated to 1.0g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 80% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 80% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 80% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 10 times of amounts of 90% ethanol lixiviate 2 times, each 2 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 2g medical material/ml with hot water, add hydrochloric acid and regulate PH to 1.5, cold preservation 20 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 65% ethanol recrystallization repeatedly with water washing;
(3) get bilobalide, breviscapine and commercially available ligustrazine hydrochloride, add pharmaceutic adjuvant, make lyophilized injectable powder, be used for the treatment of angina pectoris.
Embodiment 17.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 20;
Breviscapine 60;
Ligustrazine hydrochloride 20.
Its preparation method is,
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 9 times of water gagings and decocts 2 times, each 3 hours, merge decocting liquid, and put and be chilled to room temperature, added suitable adsorbent stirring and adsorbing 40 hours, leave standstill filtration, collect adsorbent.Adsorbent adds 9 times of 85% ethanol amount backflow eluting, each 2 hours, filter, eluent merges, and is evaporated to 2g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 90% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 90% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 90% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 11 times of amounts of 80% ethanol lixiviate 2 times, each 1 hour, collect alcohol extract and be evaporated to thick paste, be diluted to 1g medical material/ml with hot water, add hydrochloric acid and regulate PH to 2.5, cold preservation 20 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 75% ethanol recrystallization repeatedly with water washing;
(3) get bilobalide, breviscapine and the ligustrazine hydrochloride that extracts of technology routinely, add pharmaceutic adjuvant, make slow releasing agent, be used for the treatment of angina pectoris.
Embodiment 18.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 20;
Breviscapine 20;
Ligustrazine hydrochloride 60.
Its preparation method is,
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 11 times of water gagings and decocts 2 times, each 3 hours, merge decocting liquid, and put and be chilled to room temperature, added suitable adsorbent stirring and adsorbing 48 hours, leave standstill filtration, collect adsorbent.Adsorbent adds 9 times of 75% ethanol amount backflow eluting, each 2 hours, filter, eluent merges, and is evaporated to 1.5g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 65% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 65% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 65% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 7 times of amounts of 80% ethanol lixiviate 3 times, each 3 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 2g medical material/ml with hot water, add hydrochloric acid and regulate PH to 3, cold preservation 12 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 70% ethanol recrystallization repeatedly with water washing;
(3) get bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, make controlled release preparation, be used for the treatment of angina pectoris.
Embodiment 19.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 50;
Breviscapine 25;
Ligustrazine hydrochloride 25.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made infusion solution routinely, is used for the treatment of angina pectoris.
Embodiment 20.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 25;
Breviscapine 50;
Ligustrazine hydrochloride 25.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made tablet routinely, is used for the treatment of angina pectoris.
Embodiment 21.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 25;
Breviscapine 25;
Ligustrazine hydrochloride 50.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made oral liquid routinely, is used for the treatment of angina pectoris.
Embodiment 22.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 30;
Breviscapine 30;
Ligustrazine hydrochloride 40.
Its preparation method is,
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 6 times of water gagings and decocts 2 times, each 1 hour, merge decocting liquid, and put and be chilled to room temperature, added suitable adsorbent stirring and adsorbing 12 hours, leave standstill filtration, collect adsorbent.Adsorbent adds 6 times of 50% ethanol amount backflow eluting, each 1 hour, filter, eluent merges, and is evaporated to 0.5g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 60% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 60% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 60% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 6 times of amounts of 75% ethanol lixiviate 2 times, each 3 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1g medical material/ml with hot water, add hydrochloric acid and regulate PH to 1, cold preservation 12 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 60% ethanol recrystallization repeatedly with water washing;
(3) get the ligustrazine hydrochloride that bilobalide, breviscapine and common process extract, add pharmaceutic adjuvant, make the extractum sheet, be used for the treatment of angina pectoris.
Embodiment 23.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 30;
Breviscapine 40;
Ligustrazine hydrochloride 30.
Its preparation method is,
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 12 times of water gagings and decocts 3 times, each 1 hour, merge decocting liquid, and put and be chilled to room temperature, added suitable adsorbent stirring and adsorbing 48 hours, leave standstill filtration, collect adsorbent.Adsorbent adds 10 times of 95% ethanol amount backflow eluting, each 3 hours, filter, eluent merges, and is evaporated to 2g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 95% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 95% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 95% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 12 times of amounts of 95% ethanol lixiviate 3 times, each 1 hour, collect alcohol extract and be evaporated to thick paste, be diluted to 2g medical material/ml with hot water, add hydrochloric acid and regulate PH to 3, cold preservation 36 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 80% ethanol recrystallization repeatedly with water washing;
(3) get bilobalide, breviscapine and commercially available ligustrazine hydrochloride, add pharmaceutic adjuvant, make injection, be used for the treatment of angina pectoris.
Embodiment 24.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 40;
Breviscapine 30;
Ligustrazine hydrochloride 30.
Its preparation method is;
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 9 times of water gagings and decocts 2 times, each 2 hours, merge decocting liquid, and put and be chilled to room temperature, add active carbon or chromatographic silica gel and made the adsorbent stirring and adsorbing 24 hours, leave standstill filtration, collect adsorbent; Adsorbent adds 8 times of 70% ethanol amount backflow eluting, each 2 hours, filter, eluent merges, and is evaporated to 1g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 80% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 80% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 80% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 9 times of amounts of 85% ethanol lixiviate 2 times, each 2 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1.5g medical material/ml with hot water, add hydrochloric acid and regulate PH to 2, cold preservation 24 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 70% ethanol recrystallization repeatedly with water washing;
(3) get bilobalide, breviscapine and, add pharmaceutic adjuvant, make injection by 452 pages of described ligustrazine hydrochloride of Chinese Pharmacopoeia in 1977.
Embodiment 25.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 30;
Breviscapine 40;
Ligustrazine hydrochloride 40.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made Extencap routinely, is used for the treatment of angina pectoris.
Embodiment 26.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 30;
Breviscapine 30;
Ligustrazine hydrochloride 30.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made capsule routinely, is used for the treatment of angina pectoris.
Embodiment 27.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 40;
Breviscapine 40;
Ligustrazine hydrochloride 40.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made tablet routinely, is used for the treatment of angina pectoris.
Embodiment 28.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 40;
Breviscapine 40;
Ligustrazine hydrochloride 30.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made drop pill routinely, is used for the treatment of angina pectoris.
Embodiment 29.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 30;
Breviscapine 35;
Ligustrazine hydrochloride 35.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made Extencap routinely, is used for the treatment of angina pectoris.
Embodiment 30.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 35;
Breviscapine 30;
Ligustrazine hydrochloride 35.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made capsule routinely, is used for the treatment of angina pectoris.
Embodiment 31.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 35;
Breviscapine 35;
Ligustrazine hydrochloride 30.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made Extencap routinely, is used for the treatment of angina pectoris.
Embodiment 32.A kind of vein-relaxing pain-relieving medicinal composition Extencap, the weight proportion of raw material consists of,
Bilobalide 20; Breviscapine 10; Ligustrazine hydrochloride 70.
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 6 times of water gagings and decocts 3 times, each 3 hours, merge decocting liquid, and put and be chilled to room temperature, add active carbon or chromatographic silica gel and made the adsorbent stirring and adsorbing 24 hours, leave standstill filtration, collect adsorbent; Adsorbent adds 10 times of 60% ethanol amount backflow eluting, each 3 hours, filter, eluent merges, and is evaporated to 2g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 95% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 95% second ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 95% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 6 times of amounts of 90% ethanol lixiviate 3 times, each 2 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1.5g medical material/ml with hot water, add hydrochloric acid and regulate PH to 2.5, cold preservation 30 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 75% ethanol recrystallization repeatedly with water washing;
(3) ligustrazine hydrochloride, commercially available quality standard are contained material in 452 pages of the Chinese Pharmacopoeias in 1977;
(4) get said extracted thing and ligustrazine hydrochloride, add pharmaceutic adjuvant, add adjuvant, prepare controlled release granule, get granule, incapsulate with proper method.
Embodiment 33.A kind of vein-relaxing pain-relieving medicinal composition lyophilized injectable powder, the weight proportion of raw material consists of,
Bilobalide 70; Breviscapine 20; Ligustrazine hydrochloride 10.
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 12 times of water gagings and decocts 3 times, each 2 hours, merge decocting liquid, and put and be chilled to room temperature, add active carbon or chromatographic silica gel and made the adsorbent stirring and adsorbing 20 hours, leave standstill filtration, collect adsorbent; Adsorbent adds 10 times of 85% ethanol amount backflow eluting, each 2 hours, filter, eluent merges, and is evaporated to 1.5g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 65% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 65% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 65% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 8 times of amounts of 95% ethanol lixiviate 3 times, each 2 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1g medical material/ml with hot water, add hydrochloric acid and regulate PH to 1.4, cold preservation 16 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 80% ethanol recrystallization repeatedly with water washing;
(3) ligustrazine hydrochloride, commercially available quality standard are contained material in 452 pages of the Chinese Pharmacopoeias in 1977;
(4) get said extracted thing and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made freeze-dried powder routinely.
Embodiment 34.A kind of vein-relaxing pain-relieving medicinal composition lyophilized injectable powder, the weight proportion of raw material consists of,
Bilobalide 10; Breviscapine 70; Ligustrazine hydrochloride 20.
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 10 times of water gagings and decocts 2 times, each 3 hours, merge decocting liquid, and put and be chilled to room temperature, add active carbon or chromatographic silica gel and made the adsorbent stirring and adsorbing 24 hours, leave standstill filtration, collect adsorbent; Adsorbent adds 10 times of 75% ethanol amount backflow eluting, each 3 hours, filter, eluent merges, and is evaporated to 2g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 90% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 90% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 90% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 6 times of amounts of 80% ethanol lixiviate 3 times, each 3 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1.5g medical material/ml with hot water, add hydrochloric acid and regulate PH to 2, cold preservation 30 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 70% ethanol recrystallization repeatedly with water washing;
(3) ligustrazine hydrochloride, commercially available quality standard are contained material in 452 pages of the Chinese Pharmacopoeias in 1977;
(4) get said extracted thing and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made freeze-dried powder routinely.
Embodiment 35.A kind of vein-relaxing pain-relieving medicinal composition drop pill, the weight proportion of raw material consists of,
Bilobalide 20; Breviscapine 10; Ligustrazine hydrochloride 70.
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 8 times of water gagings and decocts 2 times, each 3 hours, merge decocting liquid, and put and be chilled to room temperature, add active carbon or chromatographic silica gel and made the adsorbent stirring and adsorbing 24 hours, leave standstill filtration, collect adsorbent; Adsorbent adds 8 times of 85% ethanol amount backflow eluting, each 2 hours, filter, eluent merges, and is evaporated to 1g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 60% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 60% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 60% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 8 times of amounts of 75% ethanol lixiviate 2 times, each 3 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1.5g medical material/ml with hot water, add hydrochloric acid and regulate PH to 2, cold preservation 12 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 70% ethanol recrystallization repeatedly with water washing;
(3) ligustrazine hydrochloride, commercially available quality standard are contained material in 452 pages of the Chinese Pharmacopoeias in 1977;
(4) get said extracted thing and ligustrazine hydrochloride, add pharmaceutic adjuvant, add in the PEG mixture, stir evenly, drip and make ball.
Embodiment 36.A kind of vein-relaxing pain-relieving medicinal composition Extencap, the weight proportion of raw material consists of,
Bilobalide 50; Breviscapine 20; Ligustrazine hydrochloride 30.
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 12 times of water gagings and decocts 2 times, each 3 hours, merge decocting liquid, and put and be chilled to room temperature, add active carbon or chromatographic silica gel and made the adsorbent stirring and adsorbing 36 hours, leave standstill filtration, collect adsorbent; Adsorbent adds 8 times of 90% ethanol amount backflow eluting, each 2 hours, filter, eluent merges, and is evaporated to 0.5g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 80% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 80% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 80% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 10 times of amounts of 80% ethanol lixiviate 2 times, each 3 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1g medical material/ml with hot water, add hydrochloric acid and regulate PH to 1.5, cold preservation 24 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 70% ethanol recrystallization repeatedly with water washing;
(3) ligustrazine hydrochloride, commercially available quality standard are contained material in 452 pages of the Chinese Pharmacopoeias in 1977;
(4) get said extracted thing and ligustrazine hydrochloride, add pharmaceutic adjuvant, add adjuvant, prepare controlled release granule, get granule, incapsulate with proper method.
Embodiment 37.A kind of vein-relaxing pain-relieving medicinal composition tablet, the weight proportion of raw material consists of,
Bilobalide 20; Breviscapine 30; Ligustrazine hydrochloride 50.
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 12 times of water gagings and decocts 2 times, each 1 hour, merge decocting liquid, and put and be chilled to room temperature, added suitable adsorbent stirring and adsorbing 12 hours, leave standstill filtration, collect adsorbent.Adsorbent adds 6 times of 65% ethanol amount backflow eluting, each 3 hours, filter, eluent merges, and is evaporated to 0.5g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 85% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 85% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 85% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 10 times of amounts of 80% ethanol lixiviate 2 times, each 2 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1.5g medical material/ml with hot water, add hydrochloric acid and regulate PH to 2, cold preservation 24 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 65% ethanol recrystallization repeatedly with water washing;
(3) ligustrazine hydrochloride, commercially available quality standard are contained material in 452 pages of the Chinese Pharmacopoeias in 1977;
(4) get said extracted thing and ligustrazine hydrochloride, add pharmaceutic adjuvant, granulate, tabletting, promptly.
Embodiment 38.A kind of vein-relaxing pain-relieving medicinal composition tablet, the weight proportion of raw material consists of,
Bilobalide 50; Breviscapine 30; Ligustrazine hydrochloride 20.
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 10 times of water gagings and decocts 3 times, each 1 hour, merge decocting liquid, and put and be chilled to room temperature, added suitable adsorbent stirring and adsorbing 24 hours, leave standstill filtration, collect adsorbent.Adsorbent adds 8 times of 75% ethanol amount backflow eluting, each 2 hours, filter, eluent merges, and is evaporated to 1g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 90% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 90% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 90% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 6 times of amounts of 75% ethanol lixiviate 3 times, each 3 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1g medical material/ml with hot water, add hydrochloric acid and regulate PH to 2.5, cold preservation 30 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 70% ethanol recrystallization repeatedly with water washing;
(3) ligustrazine hydrochloride, commercially available quality standard are contained material in 452 pages of the Chinese Pharmacopoeias in 1977;
(4) get said extracted thing and ligustrazine hydrochloride, add pharmaceutic adjuvant, granulate, tabletting, promptly.
Embodiment 39.A kind of vein-relaxing pain-relieving medicinal composition granule, the weight proportion of raw material consists of,
Bilobalide 60; Breviscapine 25; Ligustrazine hydrochloride 15.
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 8 times of water gagings and decocts 2 times, each 3 hours, merge decocting liquid, and put and be chilled to room temperature, added suitable adsorbent stirring and adsorbing 15 hours, leave standstill filtration, collect adsorbent.Adsorbent adds 10 times of 60% ethanol amount backflow eluting, each 3 hours, filter, eluent merges, and is evaporated to 2g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 80% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 80% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 80% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 12 times of amounts of 75% ethanol lixiviate 3 times, each 2 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1g medical material/ml with hot water, add hydrochloric acid and regulate PH to 2, cold preservation 24 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 80% ethanol recrystallization repeatedly with water washing;
(3) ligustrazine hydrochloride, commercially available quality standard are contained material in 452 pages of the Chinese Pharmacopoeias in 1977;
(4) get said extracted thing and ligustrazine hydrochloride, add pharmaceutic adjuvant, make granule, warm water is taken after mixing it with water.
Embodiment 40.A kind of vein-relaxing pain-relieving medicinal composition extract tablet, the weight proportion of raw material consists of,
Bilobalide 15; Breviscapine 60; Ligustrazine hydrochloride 25.
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 6 times of water gagings and decocts 3 times, each 2 hours, merge decocting liquid, and put and be chilled to room temperature, add active carbon or chromatographic silica gel and made the adsorbent stirring and adsorbing 30 hours, leave standstill filtration, collect adsorbent; Adsorbent adds 10 times of 60% ethanol amount backflow eluting, each 3 hours, filter, eluent merges, and is evaporated to 0.5g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 70% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 70% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 70% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 10 times of amounts of 75% ethanol lixiviate 3 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1.5g medical material/ml with hot water, add hydrochloric acid and regulate PH to 1.5, cold preservation 24 hours, collecting precipitation, extremely neutral with water washing, gained precipitation obtains breviscapine with 80% ethanol recrystallization repeatedly;
(3) ligustrazine hydrochloride, commercially available quality standard are contained material in 452 pages of the Chinese Pharmacopoeias in 1977;
(4) get the said extracted thing, add pharmaceutic adjuvant, add adjuvant, granulate tabletting.
Embodiment 41.A kind of vein-relaxing pain-relieving medicinal composition injection, the weight proportion of raw material consists of,
Bilobalide 25 and ligustrazine hydrochloride; Breviscapine 15; Ligustrazine hydrochloride 60.
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 12 times of water gagings and decocts 3 times, each 1 hour, merge decocting liquid, and put and be chilled to room temperature, add active carbon or chromatographic silica gel and made the adsorbent stirring and adsorbing 18 hours, leave standstill filtration, collect adsorbent; Adsorbent adds 10 times of 55% ethanol amount backflow eluting, each 3 hours, filter, eluent merges, and is evaporated to 1.5g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 75% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 75% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 75% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 8 times of amounts of 90% ethanol lixiviate 2 times, each 3 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1g medical material/ml with hot water, add hydrochloric acid and regulate PH to 2.5, cold preservation 15 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 65% ethanol recrystallization repeatedly with water washing;
(3) ligustrazine hydrochloride, commercially available quality standard are contained material in 452 pages of the Chinese Pharmacopoeias in 1977;
(4) get said extracted thing and ligustrazine hydrochloride, add pharmaceutic adjuvant, make injection.
Embodiment 42.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 20;
Breviscapine 20;
Ligustrazine hydrochloride 20.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made Extencap routinely, is used for the treatment of angina pectoris.
Embodiment 43.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 25;
Breviscapine 75;
Ligustrazine hydrochloride 75.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made capsule routinely, is used for the treatment of angina pectoris.
Embodiment 44.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 45;
Breviscapine 65;
Ligustrazine hydrochloride 45.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made tablet routinely, is used for the treatment of angina pectoris.
Embodiment 45.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 55;
Breviscapine 45;
Ligustrazine hydrochloride 65.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made drop pill routinely, is used for the treatment of angina pectoris.
Embodiment 46.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 65;
Breviscapine 55;
Ligustrazine hydrochloride 35.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made Extencap routinely, is used for the treatment of angina pectoris.
Embodiment 47.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 75;
Breviscapine 15;
Ligustrazine hydrochloride 55.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made capsule routinely, is used for the treatment of angina pectoris.
Embodiment 48.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 15;
Breviscapine 75;
Ligustrazine hydrochloride 35.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made Extencap routinely, is used for the treatment of angina pectoris.
Embodiment 49.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 50;
Breviscapine 50;
Ligustrazine hydrochloride 50.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made Extencap routinely, is used for the treatment of angina pectoris.
Embodiment 50.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 60;
Breviscapine 60;
Ligustrazine hydrochloride 60.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made capsule routinely, is used for the treatment of angina pectoris.
Embodiment 51.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 70;
Breviscapine 70;
Ligustrazine hydrochloride 70.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made tablet routinely, is used for the treatment of angina pectoris.
Embodiment 52.A kind of vein-relaxing pain-relieving medicinal composition, the weight proportion of raw material consists of,
Bilobalide 80;
Breviscapine 80;
Ligustrazine hydrochloride 80.
Its preparation method is, extract according to a conventional method bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, technology is made drop pill routinely, is used for the treatment of angina pectoris.
Claims (7)
1. a vein-relaxing pain-relieving medicinal composition is characterized in that, the weight proportion of raw material consists of,
Bilobalide 10～80;
Breviscapine 10～80;
Ligustrazine hydrochloride 10～80.
2. a kind of vein-relaxing pain-relieving medicinal composition according to claim 1 is characterized in that the weight proportion of raw material consists of,
Bilobalide 20～60;
Breviscapine 20～60;
Ligustrazine hydrochloride 20～60.
3. a kind of vein-relaxing pain-relieving medicinal composition according to claim 1 is characterized in that the weight proportion of raw material consists of,
Bilobalide 30～40;
Breviscapine 30～40;
Ligustrazine hydrochloride 30～40.
4. a kind of vein-relaxing pain-relieving medicinal composition according to claim 1 is characterized in that the weight proportion of raw material consists of,
Bilobalide 40;
Breviscapine 30;
Ligustrazine hydrochloride 30.
5. the preparation method as any one described vein-relaxing pain-relieving medicinal composition among the claim 1-4 is characterized in that,
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 6-12 times of water gagings and decocts 2-3 times, each 1-3 hours, merge decocting liquid, and put and be chilled to room temperature, added suitable adsorbent stirring and adsorbing 12-48 hours, leave standstill filtration, collect adsorbent.Adsorbent adds 6-10 times of amounts of 50-95% ethanol backflow eluting, each 1-3 hours, filter, eluent merges, and is evaporated to 0.5-2g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 60-95% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 60-95% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 60-95% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 6-12 times of amounts of 75-95% ethanol lixiviate 2-3 times, each 1-3 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1-2g medical material/ml with hot water, add hydrochloric acid and regulate PH to 1-3, cold preservation 12-36 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 60-80% ethanol recrystallization repeatedly with water washing;
(3) get bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, make the medicine that to accept dosage form on any pharmaceutics.
6. the preparation method of vein-relaxing pain-relieving medicinal composition according to claim 5 is characterized in that,
(1) preparation technology of bilobalide is, gets Folium Ginkgo, and fragmentation adds 9 times of water gagings and decocts 2 times, each 2 hours, merge decocting liquid, and put and be chilled to room temperature, add active carbon or chromatographic silica gel and made the adsorbent stirring and adsorbing 24 hours, leave standstill filtration, collect adsorbent; Adsorbent adds 8 times of 70% ethanol amount backflow eluting, each 2 hours, filter, eluent merges, and is evaporated to 1g medical material/ml, the cold preservation crystallize, collect separate out crystal repeatedly with 80% ethyl alcohol recrystallization to highly finished product; Above-mentioned bilobalide highly finished product are with acetone solution, and proper silica gel is mixed sample, and the silicagel column of packing into 80% ethanol elution, is collected the eluent concentrating under reduced pressure, cold preservation crystallize, gained crystallize repeatedly with 80% ethyl alcohol recrystallization to needle;
(2) preparation technology of breviscapine is, get the Herba Erigerontis Herb and be ground into coarse powder, with 9 times of amounts of 85% ethanol lixiviate 2 times, each 2 hours, collect alcohol extract and be evaporated to thick paste, be diluted to 1.5g medical material/ml with hot water, add hydrochloric acid and regulate PH to 2, cold preservation 24 hours, collecting precipitation, to neutral, the gained precipitation obtains breviscapine with 70% ethanol recrystallization repeatedly with water washing;
(3) get bilobalide, breviscapine and ligustrazine hydrochloride, add pharmaceutic adjuvant, make injection.
7. any one described a kind of vein-relaxing pain-relieving medicinal composition is preparing the purposes for the treatment of in the treating coronary heart disease and angina pectoris in the claim 1-4.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1053609A (en) * | 1990-01-25 | 1991-08-07 | 云南省生物制药厂 | The extraction process of Herba Erigerontis tablet bulk drug |
| CN1195665A (en) * | 1997-12-02 | 1998-10-14 | 周国柱 | Method for extracting ginkgo lactone and preparation containing the same |
| CN1562058A (en) * | 2004-04-01 | 2005-01-12 | 陈谨 | Medicinal composition for treating cardiocerebral diseases |
| CN1788731A (en) * | 2004-12-17 | 2006-06-21 | 秦引林 | Compound injection preparation containing ligustrazine and breviscapine and its preparation method |
-
2006
- 2006-10-19 CN CN2006100969754A patent/CN101164546B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1053609A (en) * | 1990-01-25 | 1991-08-07 | 云南省生物制药厂 | The extraction process of Herba Erigerontis tablet bulk drug |
| CN1195665A (en) * | 1997-12-02 | 1998-10-14 | 周国柱 | Method for extracting ginkgo lactone and preparation containing the same |
| CN1562058A (en) * | 2004-04-01 | 2005-01-12 | 陈谨 | Medicinal composition for treating cardiocerebral diseases |
| CN1788731A (en) * | 2004-12-17 | 2006-06-21 | 秦引林 | Compound injection preparation containing ligustrazine and breviscapine and its preparation method |
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