CN103505489A - Traditional Chinese medicine composition containing Sichuan lovage rhizome and preparation method of composition - Google Patents
Traditional Chinese medicine composition containing Sichuan lovage rhizome and preparation method of composition Download PDFInfo
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- CN103505489A CN103505489A CN201210217233.8A CN201210217233A CN103505489A CN 103505489 A CN103505489 A CN 103505489A CN 201210217233 A CN201210217233 A CN 201210217233A CN 103505489 A CN103505489 A CN 103505489A
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Abstract
The invention discloses a traditional Chinese medicine composition containing Sichuan lovage rhizome. The composition comprises the following active pharmaceutical ingredients in parts by weight: 3-30 parts of sea-buckthorn, 3-25 parts of Sichuan lovage rhizome and 5-20 parts of pseudo-ginseng. The invention also discloses a preparation method of the traditional Chinese medicine composition. The preparation method comprises the steps of extracting active ingredients and preparing the finished product according to the formula. The composition makes the best of the treatment effects of the active pharmaceutical ingredients on cardiovascular diseases, adopts scientific matching, generates synergistic effects, has good curative effects and more controllable quality and is suitable for industrial production.
Description
Technical field
The Chinese medicine composition and the preparation method that the present invention relates to a kind of Cardiovarscular, 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 the underlying cause of death of one of the disease that threat human health the is the most serious ，Shi 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 ".
The drug main for the treatment of in the market coronary heart disease will be divided into: nitrate esters medicine (as isosorbide mononitrate soft gelatin capsule), thromboembolism preventing (coagulating) medicine (as aspirin), beta-blocker (as metoprolol), angiotensin converting enzyme inhibitor (as enalapril), calcium ion antagonist (as verapamil), fat regulation medicine (as simvastatin), anticoagulation (as heparin), the eight large classes such as Thrombolytic Drugs (as recombinant glucokinase).Because coronary heart disease is chronic disease, Drug therapy is long the course for the treatment of, and long-term taking medicine can cause the serious untoward reaction such as headache, cough, stimulation gastric mucosa, hypotension, inhibition cardiac function, infringement hepatic and renal function.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 medicine composition 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 the drug composition that contains Rhizoma Chuanxiong provided by the invention, comprise the parts by weight of component of following bulk drugs:
Fructus Hippophae 3-30 part, Rhizoma Chuanxiong 3-25 part, Radix Notoginseng 5-20 part;
Preferably, in Chinese medicine composition of the present invention, comprise the parts by weight of component of following bulk drugs:
5 ~ 25 parts of Fructus Hippophaes, 7 ~ 20 parts of Rhizoma Chuanxiongs, 10 ~ 18 parts of Radix Notoginseng;
Preferred, in Chinese medicine composition of the present invention, comprise the parts by weight of component of following bulk drugs:
9 ~ 20 parts of Fructus Hippophaes, 11 ~ 18 parts of Rhizoma Chuanxiongs, 12 ~ 15 parts of Radix Notoginseng;
Further preferred, in Chinese medicine composition of the present invention, comprise the parts by weight of component of following bulk drugs:
12 ~ 18 parts of Fructus Hippophaes, 13 ~ 15 parts of Rhizoma Chuanxiongs, 12 ~ 13 parts of Radix Notoginseng;
Further preferred again, in Chinese medicine composition of the present invention, comprise the parts by weight of component of following bulk drugs:
15 parts of Fructus Hippophaes, 15 parts of Rhizoma Chuanxiongs, 12 parts of Radix Notoginseng.
The preparation method of Fructus Hippophae extract of the present invention comprises the steps:
Get Fructus Hippophae medical 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 water elution, obtain eluent I; Then with ethanol elution 2 times, the volumetric concentration of eluting ethanol is 50% ~ 60% for the first time, and the volumetric concentration of eluting ethanol is 90% ~ 95% for the second time, obtains eluent II, reclaim, and 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 60% for the first time; The volumetric concentration of eluting ethanol is 90% for the second time.
Preferred, the preparation method of Fructus Hippophae extract of the present invention comprises the following steps:
Get Fructus Hippophae medical 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 with water elution, obtain eluent I; Then with 50% ~ 60% ethanol elution, then with 90% ~ 95% ethanol elution, obtain eluent II, 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.
Concentration of alcohol described in the present invention is volumetric concentration.
In the present invention, Rhizoma Chuanxiong and Radix Notoginseng extract can be obtained on ，Ye Keyou market and be bought by prior art.Can also adopt following method preparation:
1. by Rhizoma Chuanxiong and Radix Notoginseng extracting in water 2 times, add for the first time 6 ~ 10 times of water gagings, 90 ℃～100 ℃ of temperature keep 1.5 ~ 3 hours, 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. the upper macroporous resin adsorption of filtrate, water, 20% ~ 60% ethanol eluting, 60% ~ 95% ethanol eluting for the second time for the first time, collects eluent respectively;
3. steam pressure 0.01～0.09Mpa, vacuum-0.03～-0.08Mpa, 60～80 ℃ of temperature, are concentrated into relative density 1.20～1.25g/cm
3extractum (50～55 ℃ of surveys);
4. vacuum-0.04～-0.09Mpa, 60～95 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Preferably, step 2. in ethanol elution volumetric concentration be respectively: for the first time 30% ~ 55%; For the second time 70% ~ 90%; Preferred, the volumetric concentration of eluting ethanol is respectively: for the first time 35%; For the second time 75%.
Preferably, step is middle steam pressure 0.04～0.07Mpa 3., vacuum-0.04～-0.06Mpa, and 65～75 ℃ of temperature, are concentrated into relative density 1.20～1.25g/cm
3extractum.
Preferred, step is middle steam pressure 0.05Mpa 3., vacuum-0.06Mpa, and temperature 70 C, is concentrated into relative density 1.23g/cm
3extractum.
Chinese medicine composition 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, injectable powder.
In compositions of the present invention, can also in the situation that not affecting therapeutic purposes of the present invention and effect, add arbitrarily other compositions or the component in the present invention is equal to replacement, including but not limited to that Borneolum Syntheticum, Flos Carthami, Radix Curcumae, Rhizoma Corydalis are or/and Lignum Dalbergiae Odoriferae etc.As long as add the compositions obtaining after these compositions can also reach the therapeutic effect of the present composition, be all fine.
Chinese medicine composition of the present invention makes full use of the therapeutical effect of crude drug to cardiovascular disease, carries out scientific matching, produces coordinating effect, good effect, and quality is more controlled, is applicable to suitability for industrialized production.
test example
(1) experimentation of medicine of the present invention and Flavonihippophae function of resisting myocardial ischemia
1, grouping and administration
60 of Wister male rats, body weight 245 ± 23g, is divided into 3 groups at random by body weight: normal saline matched group; The extract group of embodiment tetra-; Flavonihippophae group.Each medicine all with normal saline dilution to desired concn, dosage is 4ml/kg, tail intravenously administrable.
2, method
(1), rat experiment myocardial infarction model: animal pentobarbital sodium intraperitoneal injection of anesthesia (45mg/kg), face upward position fixing.Tracheal intubation, makes the longitudinal incision of 2cm in breastbone left side, nearly breastbone side is cut off the 3rd, the 4th and strangled cartilage, opens behind thoracic cavity, connects artificial respirator (ventilation 2ml/100g, 50 times/min).Cut off pericardium, expose heart, left anterior descending coronary artery root threading is in order to ligation, and record standard II lead electrocardiogram, stablizes 10 minutes, and following coronary artery occlusion left anterior descending branch, closes thoracic cavity.By syringe sucking-off animal throat portion secretion, make animal recover autonomous respiration.After following coronary artery occlusion 15min, intravenously administrable.After following coronary artery occlusion 4 hours, win heart, 5 of the following crosscuts of ligature, carry out NBT (NBT) dyeing, calculating myocardium Infarct area accounts for the percentage ratio of ventricle and heart area, and carries out statistical procedures (t check).
(2), in vitro langendorff heart perfusion: carry out with reference to the pharmacological experimental methodology third edition.
3, result
(1) impact on rat experiment myocardial inyaretion scope, the results are shown in Table 1.
The various extracts of table 1 on the impact of rat experiment myocardial inyaretion scope (
)
| Group | Dosage (mg/kg) | Number of animals | Infarcted region/ventricle (%) | Infarcted region/heart (%) |
| The Chinese medicine composition of embodiment tetra- | 20 | 20 | 16.87±5.21** # | 14.94±4.78** # |
| Flavonihippophae | 20 | 20 | 24.05±6.53* | 19.18±4.39* |
| Model group | ? | 20 | 35.11±6.77 | 26.62±4.55 |
Note: compare * P<0.05, * * P<0.01 with model group; Compare with Flavonihippophae group,<sup TranNum="146">#</sup>p<0.05,<sup TranNum="147">##</sup>p<0.01;
(2) impact on the dirty coronary flow of guinea-pig heart and heart rate, the results are shown in Table 2.
The various extracts of table 2 on the impact of rat heart coronary flow and heart rate (
)
| Group | Dosage (mg/ml) | Coronary flow value added (ml/min) | Heart rate attenuating value (inferior/min) |
| The Chinese medicine composition of embodiment tetra- | 20 | 12.56±1.87 ?## | 21±11 # |
| Flavonihippophae group | 20 | 8.44±1.74 | 12±6 |
Note: compare with Flavonihippophae group,<sup TranNum="178">#</sup>p<0.05,<sup TranNum="179">##</sup>p<0.01.
The result demonstration of above table 1 and table 2, medicine of the present invention and Flavonihippophae all have obvious function of resisting myocardial ischemia, and the curative effect of the present composition is better than Flavonihippophae.
(2) the clinical experiment effect for the treatment of coronary heart disease
1, experimental drug
It is product, isosorbide mononitrate, simvastatin, the Flavonihippophae of the embodiment of the present invention 4 preparations that the present invention treats 1 group.
2, object choice
Select altogether out-patient's 200 examples, be divided at random treatment group of the present invention, isosorbide mononitrate group, Flavonihippophae group, four groups of simvastatin group.
Every group of 50 examples.
Treatment group 50 examples of the present invention, male 29 examples, female's 21 examples; The oldest 78 years old, minimum 52 years old, average 69.2 years old; The shortest 5 weeks of the course of disease, the longest 19 years.
Isosorbide mononitrate group 50 examples, male 25 examples, female's 25 examples; The oldest 77 years old, minimum 51 years old, average 68.2 years old; The course of disease is the shortest 4 weeks, the longest 21 years.
Flavonihippophae group 50 examples, male 24 examples, female's 26 examples; The oldest 79 years old, minimum 51 years old, average 68.9 years old; The course of disease is the shortest 3 weeks, the longest 19 years.
Simvastatin group 50 examples, male 24 examples, female's 26 examples; The oldest 76 years old, minimum 50 years old, average 67.7 years old; The course of disease is the shortest 5 weeks, the longest 20 years.
Each is organized patient and at aspects such as sex, age, the course of disease, state of an illness weight and primary diseases, carries out harmony relatively, and no significant difference (P > 0.05), there is comparability.
3, method
Each organizes and is 3 months the course for the treatment of; Each group is all carried out detecting ECG before treatment and after treating 3 months, implements angina pectoris symptom efficacy evaluation simultaneously.Angina pectoris attacks situation, the electrocardiogram of observing all Treatment in Patients with Coronary Hearts front and back improve situation.Conventional therapy: medicine 10mg of the present invention, every day 2 times; Oral Shu Bilaite (isosorbide mononitrate soft gelatin capsule) 10mg, every day 2 times; Oral Flavonihippophae 10mg, every day 2 times; Simvastatin 20mg, 1 time every night.Complicated hypertension person gives Treatment of Hypertension simultaneously.
4, curative effect determinate standard
With reference to national Angina Pectoris from Coronary Artery Disease with Therapy of Combination of TCM with Western Medicine forum in 1979 " angina pectoris and ECG curative effect evaluation criteria ".
(1) angina pectoris symptom efficacy evaluation: effective: equal tired degree does not cause that angina pectoris or angina pectoris attacks number of times reduce more than 80%; Effective: angina pectoris attacks number of times reduces 50%～80%; Invalid: angina pectoris attacks number of times reduces less than 50%.
(2) coronary heart disease ECG curative effect evaluation: effective: electrocardiogram returns to normally; Effective: ST section reduces, after treatment, go up more than 0.05 mV, but do not reach normal level, the negative T wave that mainly leads shoals (reaching more than 25%) or T ripple becomes upright person from smooth, or chamber or intraventricular block improver; Invalid: electrocardiogram is front basic identical with treatment.
5 results
(1) respectively organize the comparison of angina pectoris symptom curative effect
After treatment, each organizes angina pectoris situation in Table 3.The curative effect for the treatment of group of the present invention is obviously better than other each groups.Through check, the total effective rate for the treatment of group of the present invention is significantly higher than other groups (P < 0.05).
(2) respectively organize the comparison of patient's ECG curative effect
Electrocardiogram improvement situation is relatively in Table 4.As can be seen from Table 4, the total effective rate for the treatment of group of the present invention is significantly better than other groups (P < 0.05).
The comparison of table 3 angina pectoris treatment situation
| Group | Number of cases | Effective | Effectively | Invalid | Effective percentage (%) |
| Treatment group of the present invention | 50 | 27 | 16 | 7 | 86.0 |
| Isosorbide mononitrate group | 50 | 21 | 17 | 12 | 76.0 |
| Flavonihippophae group | 50 | 20 | 19 | 11 | 78.0 |
| Simvastatin group | 50 | 21 | 17 | 12 | 76.0 |
Table 4 electrocardiogram improves situation comparison
| Group | Number of cases | Effective | Effectively | Invalid | Effective percentage (%) |
| Treatment group of the present invention | 50 | 28 | 16 | 6 | 88.0 |
| Isosorbide mononitrate group | 50 | 23 | 15 | 12 | 76.0 |
| Flavonihippophae group | 50 | 22 | 17 | 11 | 78.0 |
| Simvastatin group | 50 | 22 | 17 | 11 | 78.0 |
As can be known from the above table, each organize medicine all have treatment anginal effect, treatment group better efficacy of the present invention.
The specific embodiment
embodiment 1
According to following weight portion, get each raw material effective component extracting: 3 parts of Fructus Hippophaes, 3 parts of Rhizoma Chuanxiongs, 5 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 1 hour for the first time, 1 hour for the second time, filtrate merged 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, adopt macroporous resin AB-8 to carry out separation to it, first with water elution, obtain eluent I; Then with 50% ethanol elution, then with 90% ethanol elution, elution flow rate is 1BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 2
According to following weight portion, get each raw material effective component extracting: 30 parts of Fructus Hippophaes, 25 parts of Rhizoma Chuanxiongs, 20 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 3 hours for the first time, 2 hours for the second time, filtrate merged 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, adopt macroporous resin X-5 to carry out separation to it, first with water elution, obtain eluent I; Then with 60% ethanol elution, then with 95% ethanol elution, elution flow rate is 4BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 3
According to following weight portion, get each raw material effective component extracting: 5 parts of Fructus Hippophaes, 7 parts of Rhizoma Chuanxiongs, 10 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 1.5 hours for the first time, 1.5 hours for the second time, filtrate merged 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, adopt macroporous resin AB-8 to carry out separation to it, first with water elution, obtain eluent I; Then with 55% ethanol elution, then with 95% ethanol elution, elution flow rate is 3BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 4
According to following weight portion, get each raw material effective component extracting: 15 parts of Fructus Hippophaes, 15 parts of Rhizoma Chuanxiongs, 12 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 3 hours for the first time, 1 hour for the second time, filtrate merged 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, adopt macroporous resin X-5 to carry out separation to it, first with water elution, obtain eluent I; Then with 60% ethanol elution, then with 90% ethanol elution, elution flow rate is 2BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 5
According to following weight portion, get each raw material effective component extracting: 25 parts of Fructus Hippophaes, 20 parts of Rhizoma Chuanxiongs, 18 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 3 hours for the first time, 1 hour for the second time, filtrate merged 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, adopt macroporous resin X-5 to carry out separation to it, first with water elution, obtain eluent I; Then with 55% ethanol elution, then with 95% ethanol elution, elution flow rate is 2BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 6
According to following weight portion, get each raw material effective component extracting: 9 parts of Fructus Hippophaes, 11 parts of Rhizoma Chuanxiongs, 12 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 2 hours for the first time, 1 hour for the second time, filtrate merged 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, adopt macroporous resin AB-8 to carry out separation to it, first with water elution, obtain eluent I; Then with 58% ethanol elution, then with 94% ethanol elution, elution flow rate is 3BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 7
According to following weight portion, get each raw material effective component extracting: 20 parts of Fructus Hippophaes, 18 parts of Rhizoma Chuanxiongs, 15 parts of Radix Notoginseng.
(1) Fructus Hippophae medical material is got in the preparation of Fructus Hippophae extract, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating extraction 2 times, 2.5 hours for the first time, 1.5 hours for the second time, filtrate merged to obtain extracting solution I, and 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, adopt macroporous resin X-5 to carry out separation to it, first with water elution, obtain eluent I; Then with 54% ethanol elution, then with 92% ethanol elution, elution flow rate is 1.5BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 8
According to following weight portion, get each raw material effective component extracting: 12 parts of Fructus Hippophaes, 13 parts of Rhizoma Chuanxiongs, 12 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 3 hours for the first time, 2 hours for the second time, filtrate merged 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, adopt macroporous resin AB-8 to carry out separation to it, first with water elution, obtain eluent I; Then with 59% ethanol elution, then with 95% ethanol elution, elution flow rate is 3.5BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 9
According to following weight portion, get each raw material effective component extracting: 18 parts of Fructus Hippophaes, 15 parts of Rhizoma Chuanxiongs, 13 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 1 hour for the first time, 2 hours for the second time, filtrate merged 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, adopt macroporous resin X-5 to carry out separation to it, first with water elution, obtain eluent I; Then with 51% ethanol elution, then with 91% ethanol elution, elution flow rate is 2.5BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 10
According to following weight portion, get each raw material effective component extracting: 25 parts of Fructus Hippophaes, 25 parts of Rhizoma Chuanxiongs, 18 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 1.5 hours for the first time, 1.5 hours for the second time, filtrate merged 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, adopt macroporous resin AB-8 to carry out separation to it, first with water elution, obtain eluent I; Then with 56% ethanol elution, then with 94% ethanol elution, elution flow rate is 4BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 11
According to following weight portion, get each raw material effective component extracting: 30 parts of Fructus Hippophaes, 20 parts of Rhizoma Chuanxiongs, 20 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 3 hours for the first time, 2 hours for the second time, filtrate merged 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, adopt macroporous resin X-5 to carry out separation to it, first with water elution, obtain eluent I; Then with 60% ethanol elution, then with 90% ethanol elution, elution flow rate is 2BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 12
According to following weight portion, get each raw material effective component extracting: 10 parts of Fructus Hippophaes, 10 parts of Rhizoma Chuanxiongs, 10 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 2.5 hours for the first time, 1 hour for the second time, filtrate merged to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1.2 hours for the first time, 0.8 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 macroporous resin AB-8 to carry out separation to it, first with water elution, obtain eluent I; Then with 50% ethanol elution, then with 95% ethanol elution, elution flow rate is 3BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 13
According to following weight portion, get each raw material effective component extracting: 20 parts of Fructus Hippophaes, 15 parts of Rhizoma Chuanxiongs, 10 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 1 hour for the first time, 2 hours for the second time, filtrate merged 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, adopt macroporous resin X-5 to carry out separation to it, first with water elution, obtain eluent I; Then with 57% ethanol elution, then with 92% ethanol elution, elution flow rate is 2.2BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 14
According to following weight portion, get each raw material effective component extracting: 20 parts of Fructus Hippophaes, 12 parts of Rhizoma Chuanxiongs, 10 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 1 hour for the first time, 2 hours for the second time, filtrate merged 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, adopt macroporous resin AB-8 to carry out separation to it, first with water elution, obtain eluent I; Then with 50% ethanol elution, then with 90% ethanol elution, elution flow rate is 3.5BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 15
According to following weight portion, get each raw material effective component extracting: 10 parts of Fructus Hippophaes, 15 parts of Rhizoma Chuanxiongs, 20 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 3 hours for the first time, 2 hours for the second time, filtrate merged to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 0.5 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, adopt macroporous resin X-5 to carry out separation to it, first with water elution, obtain eluent I; Then with 60% ethanol elution, then with 90% ~ 95% ethanol elution, elution flow rate is 3BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 16
According to following weight portion, get each raw material effective component extracting: 18 parts of Fructus Hippophaes, 9 parts of Rhizoma Chuanxiongs, 10 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 2.4 hours for the first time, 1.8 hours for the second time, filtrate merged to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 0.8 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, adopt macroporous resin AB-8 to carry out separation to it, first with water elution, obtain eluent I; Then with 60% ethanol elution, then with 90% ethanol elution, elution flow rate is 1BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 17
According to following weight portion, get each raw material effective component extracting: 15 parts of Fructus Hippophaes, 5 parts of Rhizoma Chuanxiongs, 5 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 3 hours for the first time, 2 hours for the second time, filtrate merged to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 0.51 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 macroporous resin X-5 to carry out separation to it, first with water elution, obtain eluent I; Then with 55% ethanol elution, then with 90% ethanol elution, elution flow rate is 2.5BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 18
According to following weight portion, get each raw material effective component extracting: 9 parts of Fructus Hippophaes, 4 parts of Rhizoma Chuanxiongs, 5 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 2.5 hours for the first time, 1 hour for the second time, filtrate merged to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 0.6 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 macroporous resin X-5 to carry out separation to it, first with water elution, obtain eluent I; Then with 60% ethanol elution, then with 95% ethanol elution, elution flow rate is 4BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 19
According to following weight portion, get each raw material effective component extracting: 30 parts of Fructus Hippophaes, 20 parts of Rhizoma Chuanxiongs, 15 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 1 hour for the first time, 1 hour for the second time, filtrate merged to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1.5 hours for the first time, 0.6 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 macroporous resin AB-8 to carry out separation to it, first with water elution, obtain eluent I; Then with 58% ethanol elution, then with 94% ethanol elution, elution flow rate is 3.5BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng extract
By raw material extracting in water 2 times, add for the first time 7 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 0.5 hour, filter merging filtrate; Macroporous adsorbent resin on filtrate, first washes with water, then uses 51% ethanol elution, and then uses 75% ethanol elution, collects eluent; Steam pressure 0.05Mpa, vacuum-0.05Mpa, 65 ℃ of temperature, are concentrated into relative density 1.25g/cm
3extractum; Vacuum-0.05Mpa, 65 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 20
According to following weight portion, get each raw material effective component extracting: 21 parts of Fructus Hippophaes, 17 parts of Rhizoma Chuanxiongs, 13 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and 70% ethanol of volume ratio 1:2, heating extraction 2 times, 3 hours for the first time, 2 hours for the second time, filtrate merged 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, adopt macroporous resin AB-8 to carry out separation to it, first with water elution, obtain eluent I; Then with 55% ethanol elution, then with 95% ethanol elution, elution flow rate is 1.5BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 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 washes with water, then uses 20% 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 1.20g/cm
3extractum; Vacuum-0.04Mpa, temperature 60 C, dry, pulverize 60 mesh sieves, obtained.
Get by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 21
According to following weight portion, get each raw material effective component extracting: 23 parts of Fructus Hippophaes, 13 parts of Rhizoma Chuanxiongs, 11 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical 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 water elution, obtain eluent I; Then with ethanol elution 2 times, the volumetric concentration of eluting ethanol is 50% ~ 60% for the first time, and the volumetric concentration of eluting ethanol is 90% ~ 95% for the second time, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 washes with water, then uses 60% ethanol elution, and then uses 78% 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 by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 22
According to following weight portion, get each raw material effective component extracting: 18 parts of Fructus Hippophaes, 15 parts of Rhizoma Chuanxiongs, 10 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, adding volume ratio is ethyl acetate and the ethanol of 1:2, 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 water elution, obtain eluent I; Then with ethanol elution 2 times, the volumetric concentration of eluting ethanol is 55% for the first time, and the volumetric concentration of eluting ethanol is 90% for the second time, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng extract
By raw material extracting in water 2 times, add for the first time 9 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 1.5 hours, filter merging filtrate; Macroporous adsorbent resin on filtrate, first washes with water, then uses 55% ethanol elution, and then uses 90% ethanol elution, collects eluent; Steam pressure 0.01Mpa, vacuum-0.03Mpa, 80 ℃ of temperature, are concentrated into relative density 1.23g/cm
3extractum; Vacuum-0.05Mpa, 95 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 23
According to following weight portion, get each raw material effective component extracting: 12 parts of Fructus Hippophaes, 7 parts of Rhizoma Chuanxiongs, 20 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, adding volume ratio is ethyl acetate and the ethanol of 1:2, 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 water elution, obtain eluent I; Then with ethanol elution 2 times, the volumetric concentration of eluting ethanol is 60% for the first time, and the volumetric concentration of eluting ethanol is 90% for the second time, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 1.5 hours, filter merging filtrate; Macroporous adsorbent resin on filtrate, first washes with water, then uses 60% ethanol elution, and then uses 80% ethanol elution, collects eluent; Steam pressure 0.09Mpa, vacuum-0.08Mpa, 80 ℃ of temperature, are concentrated into relative density 1.23g/cm
3extractum; Vacuum-0.04Mpa, 95 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
embodiment 24
According to following weight portion, get each raw material effective component extracting: 5 parts of Fructus Hippophaes, 20 parts of Rhizoma Chuanxiongs, 15 parts of Radix Notoginseng.
(1) preparation of Fructus Hippophae extract
Get Fructus Hippophae medical material, after being pulverized, adding volume ratio is ethyl acetate and the ethanol of 1:2, 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 water elution, obtain eluent I; Then with ethanol elution 2 times, the volumetric concentration of eluting ethanol is 55% for the first time, and the volumetric concentration of eluting ethanol is 95% for the second time, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain.
(2) preparation of Rhizoma Chuanxiong and Radix Notoginseng 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 hours, filter; Add for the second time 5 times of water gagings, 90 ℃～100 ℃ maintenances of temperature 1 hour, filter merging filtrate; Macroporous adsorbent resin on filtrate, first washes with water, then uses 30% ethanol elution, and then uses 65% 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, 85 ℃ of temperature, dry, pulverize 60 mesh sieves, obtained.
Get by weight ratio said medicine extract, add adjuvant and be prepared into Chinese medicine composition of the present invention.
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 Rhizoma Chuanxiong, comprises the components by weight percent of following bulk drugs: 3 ~ 30 parts of Fructus Hippophaes, 3 ~ 25 parts of Rhizoma Chuanxiongs, 5 ~ 20 parts of Radix Notoginseng.
2. Chinese medicine composition according to claim 1, is characterized in that, the weight proportion of described crude drug is: 5 ~ 25 parts of Fructus Hippophaes, 7 ~ 20 parts of Rhizoma Chuanxiongs, 10 ~ 18 parts of Radix Notoginseng.
3. Chinese medicine composition according to claim 1, is characterized in that, the weight proportion of described crude drug is: 9 ~ 20 parts of Fructus Hippophaes, 11 ~ 18 parts of Rhizoma Chuanxiongs, 12 ~ 15 parts of Radix Notoginseng.
4. Chinese medicine composition according to claim 1, is characterized in that, the weight proportion of described crude drug is: 12 ~ 18 parts of Fructus Hippophaes, 13 ~ 15 parts of Rhizoma Chuanxiongs, 12 ~ 13 parts of Radix Notoginseng; Optimum proportioning is: 15 parts of Fructus Hippophaes, 15 parts of Rhizoma Chuanxiongs, 12 parts of Radix Notoginseng.
5. a preparation method for the Chinese medicine composition described in claim 1 ~ 4, comprises the steps:
(1) get Fructus Hippophae medical 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 water elution, obtain eluent I; Then with ethanol elution 2 times, the volumetric concentration of eluting ethanol is 50% ~ 60% for the first time, and the volumetric concentration of eluting ethanol is 90% ~ 95% for the second time, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain;
(2) prepare Rhizoma Chuanxiong and Radix Notoginseng extract or the Rhizoma Chuanxiong of buying and Radix Notoginseng extract, according to formula, add the extract of step (1), add adjuvant and be prepared into Chinese medicine composition of the present invention.
6. the preparation method of Chinese medicine composition according to claim 5, is characterized in that, the volume ratio of the ethyl acetate described in step (1) and ethanol is 1:2; The volumetric concentration of the described ethanol of eluting is for the first time 60%; The volumetric concentration of eluting ethanol is 90% for the second time.
7. according to the preparation method of the Chinese medicine composition described in claim 5 or 6, it is characterized in that, the preparation method of the extract described in step (1) is: get Fructus Hippophae medical 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 merges to obtain extracting solution I, 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 merges 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 with water elution, obtain eluent I, then with 50% ~ 60% ethanol elution, then with 90% ~ 95% ethanol elution, obtain eluent II, reclaim, concentrating under reduced pressure, dry, obtain.
8. according to the preparation method of the Chinese medicine composition described in claim 5 ~ 7, it is characterized in that, the elution flow rate described in step (1) 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; The volumetric concentration of the described ethanol of eluting is for the first time 60%; The volumetric concentration of eluting ethanol is 90% for the second time.
9. according to the preparation method of the Chinese medicine composition described in claim 5 ~ 8, it is characterized in that, described Rhizoma Chuanxiong and the Radix Notoginseng extract preparation method of step (2) comprises the steps:
1. by Rhizoma Chuanxiong and Radix Notoginseng 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 hours, 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. the upper macroporous resin adsorption of filtrate, water, 20% ~ 60% ethanol eluting, 60% ~ 95% ethanol eluting for the second time for the first time, collects eluent respectively;
3. steam pressure 0.01～0.09Mpa, vacuum-0.03～-0.08Mpa, 60～80 ℃ 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. preparation method according to claim 9, is characterized in that, step 2. in ethanol elution volumetric concentration be respectively: for the first time 30% ~ 55%; For the second time 70% ~ 90%; Preferred, the volumetric concentration of eluting ethanol is respectively: for the first time 35%; For the second time 75%;
Step is middle steam pressure 0.04～0.07Mpa 3., vacuum-0.04～-0.06Mpa, and 65～75 ℃ of temperature, are concentrated into relative density 1.20～1.25g/cm
3extractum; Preferred, steam pressure 0.05Mpa, vacuum-0.06Mpa, temperature 70 C, is concentrated into relative density 1.23g/cm
3extractum.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1679704A (en) * | 2005-01-28 | 2005-10-12 | 北京阜康仁生物制药科技有限公司 | Medicinal preparation containing notoginseng and seabuckthorn fruit for cardio-cerebral blood vessel diseases and its preparing method |
| KR101027230B1 (en) * | 2002-07-31 | 2011-04-06 | 티안진 태슬리 파마슈티컬 컴퍼니 리미티드 차이나 | Composition for heart disease, method to prepare same and uses thereof |
| CN102357195A (en) * | 2011-11-04 | 2012-02-22 | 成都中医药大学 | Medicinal composition for treating cardiovascular and cerebrovascular diseases, and preparation method and application thereof |
-
2012
- 2012-06-28 CN CN201210217233.8A patent/CN103505489A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101027230B1 (en) * | 2002-07-31 | 2011-04-06 | 티안진 태슬리 파마슈티컬 컴퍼니 리미티드 차이나 | Composition for heart disease, method to prepare same and uses thereof |
| CN1679704A (en) * | 2005-01-28 | 2005-10-12 | 北京阜康仁生物制药科技有限公司 | Medicinal preparation containing notoginseng and seabuckthorn fruit for cardio-cerebral blood vessel diseases and its preparing method |
| CN102357195A (en) * | 2011-11-04 | 2012-02-22 | 成都中医药大学 | Medicinal composition for treating cardiovascular and cerebrovascular diseases, and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 黄世敬等: "《中药临床合理应用手册》", 30 April 2009 * |
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