CN104042789A - Traditional Chinese medicinal composition containing Folium Ginkgo extract, and preparation method thereof - Google Patents
Traditional Chinese medicinal composition containing Folium Ginkgo extract, and preparation method thereof Download PDFInfo
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Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a traditional Chinese medicinal composition containing a Folium Ginkgo extract. The traditional Chinese medicinal composition comprises 8-87wt% of a Folium Ginkgo extract, 2-79wt% of a grape seed extract and 10-27wt% of a natto extract. The invention also discloses a preparation method of the traditional Chinese medicinal composition. The method comprises the following steps: extracting effective components, and preparing the finished product according to a formula. The traditional Chinese medicinal composition fully utilizes the scientific proportioning of raw medicines to generate a coordinative effect, can reduce the blood fat, has better curative effect and more controllable quality than traditional preparations, and is suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of Chinese medicine composition that contains Folium Ginkgo extract and preparation method, belong to the field of Chinese medicines.
Background technology
Along with improving constantly of people's living standard, the change of dietary structure, aged tendency of population becomes clear day by day, and the sickness rate of coronary heart disease is day by day soaring.Coronary heart disease is because coronary atherosclerosis causes luminal stenosis, causes blood supply of cardiac muscle oxygen supply obstacle and the heart disease that causes, and " world killer " is known as.With regard to the whole world, since half a century, coronary heart disease has become one of disease that threat human health is the most serious, is the underlying cause of death of the U.S. and some industrialized country.According to World Health Organization's statistics, in the total death toll of the U.S., have 24.7% to die from coronary heart disease, Northern Ireland coronary heart disease case fatality rate occupies first place in the world, and is 5,36/,100,000; Japan is minimum, is 41,/10 ten thousand.In recent years, the M & M of China's coronary heart disease continues soaring, has every year at present 700,000 people of surpassing to die from coronary heart disease, is the modal a kind of cardiovascular diseases of middle-aged and elderly people, has leapt to as first of internal disease.Visible coronary heart disease has become global public hazards, and American wins cardiopathia for " pestilence in epoch ".
Hyperlipidemia is the risk factor of apoplexy, coronary heart disease, myocardial infarction, sudden death.In addition, hyperlipidemia is also to promote hypertension, an important risk factor of impaired glucose tolerance, diabetes.Hyperlipidemia also can cause fatty liver, liver cirrhosis, cholelithiasis, pancreatitis, retinal hemorrhage, blind, peripheral vascular disease, limping, hyperuricemia.So must pay much attention to the harm of hyperlipidemia, positive prevention and treatment.
Blood lipid-lowering medicine is mainly Statins in the market.Such medicine has good lipid-lowering effect, but long-term taking, can be just like myalgia, muscle inflammation, even the musclar toxicity such as rhabdomyolysis, also can produce the side effect such as internal metabolism obstacle, gastrointestinal side effect, liver loss.Meanwhile, statins price is high, and long-term taking also can the corresponding financial burden that increases patient.
So, provide controlled, cheap, the eutherapeutic pure natural plant of a kind of safety to extract medicine, there is great social meaning and economic worth.
Summary of the invention
The object of this invention is to provide a kind of good effect, the more controlled Chinese medicinal composition for reducing blood fat of quality.
Another object of the present invention is to provide a kind of preparation method of described Chinese medicine composition.
Another object of the present invention is to provide a kind ofly has the Chinese medicine composition of the market competitiveness in price equally.Described Chinese medicine composition can not increase because of the raising of curative effect patient's financial burden.
For achieving the above object, the present invention by the following technical solutions:
In drug composition of the present invention, comprise following percentage by weight component:
Folium Ginkgo extract 8%～87%, Semen Vitis viniferae extract 2%～79%, natto extract 10%～27%;
Preferably, in Chinese medicine composition of the present invention, comprise following percentage by weight component:
Folium Ginkgo extract 23%～76%, Semen Vitis viniferae extract 5%～64%, natto extract 12%～25%;
Preferred, in Chinese medicine composition of the present invention, comprise following percentage by weight component:
Folium Ginkgo extract 27%～63%, Semen Vitis viniferae extract 18%～55%, natto extract 15%～23%;
Further preferred, in Chinese medicine composition of the present invention, comprise following percentage by weight component:
Folium Ginkgo extract 35%～47%, Semen Vitis viniferae extract 33%～45%, natto extract 18%～21%;
Further preferred again, in Chinese medicine composition of the present invention, comprise following percentage by weight:
Folium Ginkgo extract 45%, Semen Vitis viniferae extract 36%, natto extract 19%.
The percentage by weight sum of Folium Ginkgo extract, Semen Vitis viniferae extract, natto extract is 100%.
In pharmaceutical composition of the present invention, Folium Ginkgo extract and natto extract can adopt respectively following method to extract, and then mix by proportioning, or Folium Ginkgo and natto raw material are mixed, then extract with following method simultaneously.
Described extracting method comprises the steps:
Get raw material, after being pulverized, add ethyl acetate and ethanol, heating and refluxing extraction, obtain extracting solution I, medicinal residues add ethanol, and heating and refluxing extraction obtains extracting solution II, merge extractive liquid, I and II, be condensed into extractum, use dissolve with ethanol extractum, adopt nonpolar or low pole macroporous resin to carry out separation to it, first with 65%～70% ethanol elution, obtain eluent I; Then with 85%～90% ethanol elution, obtain eluent II, reclaim, concentrating under reduced pressure, dry, obtain.
Preferably, the volume ratio of described ethyl acetate and ethanol is 1:2.
Preferably, the volumetric concentration of eluting ethanol is 65% for the first time; The volumetric concentration of eluting ethanol is 90% for the second time.
Preferred, in Chinese medicine composition of the present invention, the preparation method of Folium Ginkgo extract and natto extract comprises the following steps:
Get raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 1～3 hour for the first time, 1～2 hour for the second time, filtrate merged to obtain extracting solution I, and medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 0.5～1.5 hour for the first time, 0.5～1 hour for the second time, filtrate merged to obtain extracting solution II, merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopt nonpolar or low pole macroporous resin to carry out separation to it, first 65%～70% ethanol elution, obtains eluent I; With 85%～90% ethanol elution, obtain eluent II again, reclaim, concentrating under reduced pressure, dry, obtain.
Described elution flow rate is 1～4BV/h; Preferably, elution flow rate is 1～2BV/h, is more preferably 2BV/h.
Described macroporous resin is preferably AB-8 and X-5, more preferably X-5.
After testing, the total flavones product purity of Folium Ginkgo extract and natto extract can reach respectively 24～26%.
Concentration of alcohol described in the present invention is volumetric concentration.
In the present invention, Semen Vitis viniferae extract can be obtained by prior art, also can be by buying on market.Can also adopt following method preparation:
(1) by raw material extracting in water 2 times, add for the first time 6～10 times of water gagings, 90 ℃～100 ℃ of temperature keep 1.5-3 hour, filter; Add for the second time 4～8 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 0.5～1.5 hour, filter merging filtrate;
(2) macroporous adsorbent resin on filtrate, uses respectively 20%～60% ethanol eluting, 60%～95% ethanol eluting for the second time for the first time, collects eluent;
(3) steam pressure 0.01～0.09Mpa, vacuum-0.03～-0.08Mpa, 50～85 ℃ of temperature, are concentrated into relative density 1.20～1.25g/cm
3extractum (40～45 ℃ of surveys);
(4) vacuum-0.04～-0.09Mpa, 60～95 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Preferably, ethanol elution volumetric concentration is respectively in step (2): for the first time 30%～55%; For the second time 70%～80%; Preferred, the volumetric concentration of eluting ethanol is respectively: for the first time 35%; For the second time 75%.
Preferably, steam pressure 0.04～0.07Mpa in step (3), vacuum-0.04～-0.06Mpa, 65～75 ℃ of temperature, are concentrated into relative density 1.20～1.25g/cm
3extractum.
Preferred, steam pressure 0.05Mpa in step (3), vacuum-0.06Mpa, temperature 70 C, is concentrated into relative density 1.23g/cm
3extractum.
Compositions of the present invention, the various dosage forms that can be mixed as starch, dextrin, lactose, microcrystalline Cellulose, hydroxypropyl methylcellulose, Polyethylene Glycol, magnesium stearate, micropowder silica gel, xylitol, lactose, glucose, glycine, mannitol, glycine etc. with adjuvant on any or more than one pharmaceuticss, for example, can be made into aqueous injection, tablet, slow releasing tablet, drop pill, granule, injectable powder, capsule, microgranule.Preferred dosage form is drop pill, capsule.
Chinese medicine composition of the present invention makes full use of crude drug and carries out scientific matching, produces coordinating effect blood fat reducing, and more traditional preparation has better curative effect, and quality is more controlled, is applicable to suitability for industrialized production.
test example
Medicine blood fat reducing clinical observation of the present invention
1. data and method
1.1 physical data are selected hyperlipidemia patient 80 examples at random, male 41 examples, and female's 39 examples, at 46.8～74.9 years old age, average 57.9 years old, alternative 80 routine hyperlipidemia patients were matched group, male 40 examples, female's 40 examples, 46.4～74.7 years old age, 58.5 years old mean age.
1.2 administrated method
Treatment group adopts the embodiment of the present invention 3 medicines, each 10mg, oral 3 times of every day, 2 months courses for the treatment of.Matched group gives Xuezhikang, each 10mg, every day 3 times, 2 months courses for the treatment of.Before treatment, withdraw other hypolipidemic.All patients before treatment, treatment does hematuria routine, blood fat, liver function, renal function, serum potassium, uranium, chlorine, blood glucose, Electrocardioscopy after January and the course for the treatment of finishing.
1.3 observation item
Before and after treatment, take out limosis vein blood and detect serum total cholesterol (TC), triglyceride (TG), high density lipoprotein (HDL-C), low density lipoprotein, LDL (LDL-C), do liver function, renal function, blood, urine routine test simultaneously.
1.4 statistical procedures
Mean ± standard deviation for measurement data (
) represent, adopt t check; Enumeration data is checked with x2, and P < 0.05 has significance for difference.
2. result
Before and after table 1 liang group lipid therapy, compare (
)
Before and after note: * group internal therapy, than P<0.01, between # group, after treatment, compare P<0.01.
The present invention and Xuezhikang all have lipid-lowering effect, and present composition lipid-lowering effect is better than Xuezhikang.
The specific embodiment
embodiment 1
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with methanol extractum, adopts macroporous resin AB-8 to carry out separation, first with 65% ethanol elution, obtains eluent I; With 85% ethanol elution, eluent flow rate is 2.5BV/h again, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 6 times of water gagings, 90 ℃～100 ℃ of temperature keep 1.5 hours, filter; Add for the second time 4 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 0.5 hour, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 20% ethanol elution, and then with 60%～95% ethanol elution, collects eluent; Steam pressure 0.01Mpa, vacuum-0.03Mpa, temperature 60 C, is concentrated into relative density 1.20g/cm
3extractum; Vacuum-0.04Mpa, temperature 60 C, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 87g, Semen Vitis viniferae extract 3g, natto extract 10g, adds adjuvant to make 1000, tablet.
embodiment 2
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with methanol extractum, adopts macroporous resin X-5 to carry out separation, first with 70% ethanol elution, obtains eluent I; With 90% ethanol elution, eluent flow rate is 2BV/h again, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 10 times of water gagings, 90 ℃～100 ℃ of temperature keep 3 hours, filter; Add for the second time 8 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 1.5 hours, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 60% ethanol elution, and then uses 95% ethanol elution, collects eluent; Steam pressure 0.09Mpa, vacuum-0.08Mpa, 80 ℃ of temperature, are concentrated into relative density 1.25g/cm
3extractum; Vacuum-0.09Mpa, 95 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 8g, Semen Vitis viniferae extract 79g, natto extract 13g, adds adjuvant to make 1000 of capsules.
embodiment 3
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 2 hours for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X-5 to carry out separation, first with 65% ethanol elution, obtains eluent I; With 90% ethanol elution, eluent flow rate is 2BV/h again, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 8 times of water gagings, 90 ℃～100 ℃ of temperature keep 2 hours, filter; Add for the second time 6 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 1 hour, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 30% ethanol elution, and then uses 70% ethanol elution, collects eluent; Steam pressure 0.04Mpa, vacuum-0.04Mpa, 65 ℃ of temperature, are concentrated into relative density 1.20g/cm
3extractum; Vacuum-0.04Mpa, temperature 70 C, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 24g, Semen Vitis viniferae extract 64g, natto extract 12g, adds adjuvant to make 1000 of capsules.
embodiment 4
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 1 hour for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 0.5 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin AB-8 to carry out separation, first with 65% ethanol elution, obtains eluent I; With 90% ethanol elution, eluent flow rate is 1BV/h again, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 8 times of water gagings, 90 ℃～100 ℃ of temperature keep 2 hours, filter; Add for the second time 6 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 1 hour, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 55% ethanol elution, and then uses 90% ethanol elution, collects eluent; Steam pressure 0.07Mpa, vacuum-0.06Mpa, 75 ℃ of temperature, are concentrated into relative density 1.25g/cm
3extractum; Vacuum-0.08Mpa, 90 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 76g, Semen Vitis viniferae extract 12g, natto extract 12g, adds adjuvant to make 1000, tablet.
embodiment 5
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 3 hours for the first time, 2 hours for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X-5 to carry out separation, first with 70% ethanol elution, obtains eluent I; With 88% ethanol elution, eluent flow rate is 4BV/h again, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 8 times of water gagings, 90 ℃～100 ℃ of temperature keep 2 hours, filter; Add for the second time 6 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 1 hour, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 35% ethanol elution, and then uses 75% ethanol elution, collects eluent; Steam pressure 0.05Mpa, vacuum-0.06Mpa, temperature 70 C, is concentrated into relative density 1.23g/cm
3extractum; Vacuum-0.06Mpa, 80 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 45g, Semen Vitis viniferae extract 36g, natto extract 19g, adds adjuvant to make 1000 bags of electuaries.
embodiment 6
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X-5 to carry out separation, first with 65% ethanol elution, obtains eluent I; With 86% ethanol elution, eluent flow rate is 2BV/h again, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 10 times of water gagings, 90 ℃～100 ℃ of temperature keep 3 hours, filter; Add for the second time 8 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 1.5 hours, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 50% ethanol elution, and then uses 75% ethanol elution, collects eluent; Steam pressure 0.07Mpa, vacuum-0.06Mpa, 65 ℃ of temperature, are concentrated into relative density 1.21g/cm
3extractum; Vacuum-0.05Mpa, 75 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 27g, Semen Vitis viniferae extract 55g, natto extract 18g, adds adjuvant to make 1000, tablet.
embodiment 7
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 2 hours for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X-5 to carry out separation, first with 70% ethanol elution, obtains eluent I; With 90% ethanol elution, eluent flow rate is 3BV/h again, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 7 times of water gagings, 90 ℃～100 ℃ of temperature keep 2.5 hours, filter; Add for the second time 7 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 1.5 hours, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 30% ethanol elution, and then uses 55% ethanol elution, collects eluent; Steam pressure 0.03Mpa, vacuum-0.04Mpa, 75 ℃ of temperature, are concentrated into relative density 1.24g/cm
3extractum; Vacuum-0.07Mpa, 65 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 63g, Semen Vitis viniferae extract 18g, natto extract 19g, adds adjuvant to make 1000 of drop pill.
embodiment 8
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 2 hours for the first time, 2 hours for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin AB-8 to carry out separation, first with 67% ethanol elution, obtains eluent I; With 84% ethanol elution, eluent flow rate is 2BV/h again, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 9 times of water gagings, 90 ℃～100 ℃ of temperature keep 3 hours, filter; Add for the second time 8 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 1.5 hours, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 59% ethanol elution, and then uses 85% ethanol elution, collects eluent; Steam pressure 0.08Mpa, vacuum-0.07Mpa, 78 ℃ of temperature, are concentrated into relative density 1.20g/cm
3extractum; Vacuum-0.04Mpa, 90 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 35g, Semen Vitis viniferae extract 45g, natto extract 20g, adds adjuvant to make 1000, tablet.
embodiment 9
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1.5 hours for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 1 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X-5 to carry out separation, first with 68% ethanol elution, obtains eluent I; Then with, then with 89% ethanol elution, eluent flow rate is 2.5BV/h, obtains eluent II, reclaim, concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 6 times of water gagings, 90 ℃～100 ℃ of temperature keep 1.5 hours, filter; Add for the second time 4 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 1.5 hours, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 40% ethanol elution, and then uses 80% ethanol elution, collects eluent; Steam pressure 0.09Mpa, vacuum-0.08Mpa, temperature 60 C, is concentrated into relative density 1.25g/cm
3extractum; Vacuum-0.04Mpa, 95 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 47g, Semen Vitis viniferae extract 35g, natto extract 18g, adds adjuvant to make 1000 bags of electuaries.
embodiment 10
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 3 hours for the first time, 2 hours for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X-5 to carry out separation, first with 65% ethanol elution, obtains eluent I; With 90% ethanol elution, eluent flow rate is 2BV/h again, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 9 times of water gagings, 90 ℃～100 ℃ of temperature keep 3 hours, filter; Add for the second time 7 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 0.5 hour, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 45% ethanol elution, and then uses 75% ethanol elution, collects eluent; Steam pressure 0.04Mpa, vacuum-0.05Mpa, temperature 70 C, is concentrated into relative density 1.20g/cm
3extractum; Vacuum-0.04Mpa, temperature 60 C, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 10g, Semen Vitis viniferae extract 75g, natto extract 15g, adds adjuvant to make 1000, tablet.
embodiment 11
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 2.5 hours for the first time, 1.5 hours for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin AB-8 to carry out separation, first with 65% ethanol elution, obtains eluent I; With 89% ethanol elution, eluent flow rate is 3.5BV/h again, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 6 times of water gagings, 90 ℃～100 ℃ of temperature keep 1.5 hours, filter; Add for the second time 8 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 1 hour, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 25% ethanol elution, and then uses 85% ethanol elution, collects eluent; Steam pressure 0.01Mpa, vacuum-0.03Mpa, temperature 70 C, is concentrated into relative density 1.25g/cm
3extractum; Vacuum-0.09Mpa, 95 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 80g, Semen Vitis viniferae extract 8g, natto extract 12g, adds adjuvant to make 1000, tablet.
embodiment 12
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 2.5 hours for the first time, 1.5 hours for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1.5 hours for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X-5 to carry out separation, first with 66% ethanol elution, obtains eluent I; With 87% ethanol elution, eluent flow rate is 4BV/h again, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 8 times of water gagings, 90 ℃～100 ℃ of temperature keep 2 hours, filter; Add for the second time 8 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 1 hour, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 55% ethanol elution, and then uses 80% ethanol elution, collects eluent; Steam pressure 0.09Mpa, vacuum-0.08Mpa, 63 ℃ of temperature, are concentrated into relative density 1.21g/cm
3extractum; Vacuum-0.06Mpa, 85 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 75g, Semen Vitis viniferae extract 6g, natto extract 19g, adds adjuvant to make 1000, tablet.
embodiment 13
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 3 hours for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 0.5 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X-5 to carry out separation, first with 66% ethanol elution, obtains eluent I; With 87% ethanol elution, eluent flow rate is 3.5BV/h again, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 7 times of water gagings, 90 ℃～100 ℃ of temperature keep 1.5 hours, filter; Add for the second time 5 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 0.8 hour, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 45% ethanol elution, and then uses 65% ethanol elution, collects eluent; Steam pressure 0.07Mpa, vacuum-0.05Mpa, 78 ℃ of temperature, are concentrated into relative density 1.20g/cm
3extractum; Vacuum-0.06Mpa, 65 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 67g, Semen Vitis viniferae extract 13g, natto extract 20g, adds adjuvant to make 1000 of capsules.
embodiment 14
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 1 hour for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 0.5 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin AB-8 to carry out separation, first with 68% ethanol elution, obtains eluent I; With 85% ethanol elution, eluent flow rate is 1.5BV/h again, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 9 times of water gagings, 90 ℃～100 ℃ of temperature keep 2 hours, filter; Add for the second time 7 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 0.5 hour, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 50% ethanol elution, and then uses 95% ethanol elution, collects eluent; Steam pressure 0.09Mpa, vacuum-0.08Mpa, 80 ℃ of temperature, are concentrated into relative density 1.25g/cm
3extractum; Vacuum-0.09Mpa, 95 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 50g, Semen Vitis viniferae extract 25g, natto extract 25g, adds adjuvant to make 1000, tablet.
embodiment 15
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1.5 hours for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X-5 to carry out separation, first with 65% ethanol elution, obtains eluent I; With 95% ethanol elution, eluent flow rate is 2.5BV/h again, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 8 times of water gagings, 90 ℃～100 ℃ of temperature keep 2 hours, filter; Add for the second time 6 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 1 hour, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 60% ethanol elution, and then uses 95% ethanol elution, collects eluent; Steam pressure 0.01Mpa, vacuum-0.03Mpa, 80 ℃ of temperature, are concentrated into relative density 1.25g/cm
3extractum; Vacuum-0.09Mpa, 95 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 55g, Semen Vitis viniferae extract 27g, natto extract 18g, adds adjuvant to make 1000 of capsules.
embodiment 16
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 3 hours for the first time, 2 hours for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 1 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin AB-8 to carry out separation, first with 70% ethanol elution, obtains eluent I; With 95% ethanol elution, eluent flow rate is 3BV/h again, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 9 times of water gagings, 90 ℃～100 ℃ of temperature keep 2.5 hours, filter; Add for the second time 8 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 1.5 hours, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 60% ethanol elution, and then uses 95% ethanol elution, collects eluent; Steam pressure 0.04Mpa, vacuum-0.04Mpa, 80 ℃ of temperature, are concentrated into relative density 1.25g/cm
3extractum; Vacuum-0.08Mpa, 75 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 35g, Semen Vitis viniferae extract 38g, natto extract 27g, adds adjuvant to make 1000, tablet.
embodiment 17
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 2.5 hours for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X-5 to carry out separation, first with 68% ethanol elution, obtains eluent I; With 90% ethanol elution, eluent flow rate is 1BV/h again, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 6 times of water gagings, 90 ℃～100 ℃ of temperature keep 1.5 hours, filter; Add for the second time 4 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 0.6 hour, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 36% ethanol elution, and then uses 66% ethanol elution, collects eluent; Steam pressure 0.09Mpa, vacuum-0.05Mpa, 66 ℃ of temperature, are concentrated into relative density 1.25g/cm
3extractum; Vacuum-0.08Mpa, 90 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 20g, Semen Vitis viniferae extract 60g, natto extract 20g, adds adjuvant to make 1000, tablet.
embodiment 18
(1) Folium Ginkgo extract preparation
Get Folium Ginkgo raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 3 hours for the first time, 2 hours for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1.5 hours for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin AB-8 to carry out separation, first with 69% ethanol elution, obtains eluent I; With 85% ethanol elution, eluent flow rate is 1BV/h again, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) natto extract preparation: the same.
(3) preparation of Semen Vitis viniferae extract
By raw material extracting in water 2 times, add for the first time 6 times of water gagings, 90 ℃～100 ℃ of temperature keep 3 hours, filter; Add for the second time 4 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 1.2 hours, filter merging filtrate; Macroporous adsorbent resin on filtrate, first uses 53% ethanol elution, and then uses 85% ethanol elution, collects eluent; Steam pressure 0.01Mpa, vacuum-0.07Mpa, 65 ℃ of temperature, are concentrated into relative density 1.25g/cm
3extractum; Vacuum-0.04Mpa, 75 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get above-mentioned Folium Ginkgo extract 15g, Semen Vitis viniferae extract 75g, natto extract 10g, adds adjuvant to make 1000 of capsules.
Chinese medicine composition disclosed by the invention, those skilled in the art can extract link by change and realize.Embodiments of the invention are only the specific descriptions to technical scheme, are not the restrictions to technical scheme, and those skilled in the art all fall into protection scope of the present invention not changing the replacement done under the condition of flesh and blood of the present invention or change.
Claims (10)
1. a Chinese medicine composition that contains Folium Ginkgo extract, comprises following percentage by weight component: Folium Ginkgo extract 8%～87%, Semen Vitis viniferae extract 2%～79%, natto extract 10%～27%.
2. Chinese medicine composition according to claim 1, is characterized in that, comprises following percentage by weight component: Folium Ginkgo extract 23%～76%, Semen Vitis viniferae extract 5%～64%, natto extract 12%～25%.
3. Chinese medicine composition according to claim 2, is characterized in that, comprises following percentage by weight component: Folium Ginkgo extract 27%～63%, Semen Vitis viniferae extract 18%～55%, natto extract 15%～23%.
4. Chinese medicine composition according to claim 1, is characterized in that, comprises following percentage by weight component: Folium Ginkgo extract 35%～47%, Semen Vitis viniferae extract 33%～45%, natto extract 18%～21%;
Preferably, Folium Ginkgo extract 45%, Semen Vitis viniferae extract 36%, natto extract 19%.
5. the preparation method of the compositions described in claim 1-4, described Folium Ginkgo extract and natto extract preparation method comprise the steps:
Get raw material, after being pulverized, add ethyl acetate and ethanol, heating and refluxing extraction, obtain extracting solution I, medicinal residues add ethanol, and heating and refluxing extraction obtains extracting solution II, merge extractive liquid, I and II, be condensed into extractum, use dissolve with ethanol extractum, adopt nonpolar or low pole macroporous resin to carry out separation to it, first with 65%～70% ethanol elution, obtain eluent I; Then with 85%～90% ethanol elution, obtain eluent II, reclaim, concentrating under reduced pressure, dry, obtain.
6. preparation method according to claim 5, is characterized in that, described ethyl acetate and the volume ratio of ethanol are 1:2; The volumetric concentration of eluting ethanol is 65% for the first time; The volumetric concentration of eluting ethanol is 90% for the second time.
7. preparation method according to claim 5, is characterized in that, described Folium Ginkgo extract and natto extract preparation method comprise the steps:
Get raw material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 1～3 hour for the first time, 1～2 hour for the second time, filtrate merged to obtain extracting solution I, and medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 0.5～1.5 hour for the first time, 0.5～1 hour for the second time, filtrate merged to obtain extracting solution II, merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopt nonpolar or low pole macroporous resin to carry out separation to it, first 65%～70% ethanol elution, obtains eluent I; With 85%～90% ethanol elution, obtain eluent II again, reclaim, concentrating under reduced pressure, dry, obtain.
8. preparation method according to claim 7, is characterized in that, described elution flow rate is 1～4BV/h; Preferably, elution flow rate is 1～2BV/h, is more preferably 2BV/h;
Described macroporous resin is preferably AB-8 and X-5, more preferably X-5.
9. the preparation method of the compositions described in claim 1-4, described Semen Vitis viniferae is got thing preparation method and is comprised the steps:
(1) by raw material extracting in water 2 times, add for the first time 6～10 times of water gagings, 90 ℃～100 ℃ of temperature keep 1.5-3 hour, filter; Add for the second time 4～8 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 0.5～1.5 hour, filter merging filtrate;
(2) macroporous adsorbent resin on filtrate, uses respectively 20%～60% ethanol eluting, 60%～95% ethanol eluting for the second time for the first time, collects eluent;
(3) steam pressure 0.01～0.09Mpa, vacuum-0.03～-0.08Mpa, 50～85 ℃ of temperature, are concentrated into relative density 1.20～1.25g/cm
3extractum;
(4) vacuum-0.04～-0.09Mpa, 60～95 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
10. the preparation method of compositions claimed in claim 9, is characterized in that, ethanol elution volumetric concentration is respectively in step (2): for the first time 30%～55%; For the second time 70%～80%; Preferred, the volumetric concentration of eluting ethanol is respectively: for the first time 35%; For the second time 75%;
Preferably, steam pressure 0.04～0.07Mpa in step (3), vacuum-0.04～-0.06Mpa, 65～75 ℃ of temperature, are concentrated into relative density 1.20～1.25g/cm
3extractum;
Preferred, steam pressure 0.05Mpa in step (3), vacuum-0.06Mpa, temperature 70 C, is concentrated into relative density 1.23g/cm
3extractum.
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Application publication date: 20140917 |