CN1546507A - Cape jasmine extract , its preparing process and application - Google Patents
Cape jasmine extract , its preparing process and application Download PDFInfo
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Abstract
The invention discloses a cape jasmine extract, which is an extract containing iridoid glycoside prepared from traditional Chinese medicinal herb cape jasmine as raw material, wherein the weight percent of cape jasmine glycosides in the obtained cape jasmine extract is over 30%. The cape jasmine extract has the biological activity of treating cerebrovascular diseases. The invention also discloses the method for preparation and use.
Description
Affiliated technical field
The present invention relates to a kind of Chinese medical extract, more particularly, the present invention relates to a kind of extract that from the Chinese medicine cape jasmine, prepares. The invention still further relates to preparation method and the application in the medicine of preparation treatment cardiovascular and cerebrovascular diseases thereof of this Chinese medical extract.
Background technology
Coronary heart disease and the cerebrovascular such as cerebral infarction etc. are common disease among the elderly, frequently-occurring disease, and in developed country, in China, its M ﹠ M all is the trend that increases year by year. The illness rate of China's cardiovascular disease, the incidence of disease, the death rate continue over 30 years to rise. In recent years it is about 40% in the total death of population to add up cardiovascular and cerebrovascular diseases death, and the cardiovascular and cerebrovascular patient is died from the annual whole nation 2,000,000 people approximately, and the death rate is about 20,0/1 0 ten thousand, is higher than U.S., adds, the state such as method, day, Sweden, Switzerland. China has been cardiovascular disease state occurred frequently, the whole world has nearly 1/4th populations to be threatened by cardiovascular and relevant disease now, and throughout one's life, may have 1/3rd people's life to be shrouded by the angiocardiopathy shade, there is at last 1/5th population to die from cardiovascular related diseases.
At present the types of drugs of Cardiovarscular is more, and Chinese medicine is arranged, and chemical drugs is also arranged, although the preparation such as chemical drugs such as monobel determined curative effect wherein has various serious side effects, also produces easily drug resistance; Oral preparation of Chinese traditional medicinal such as Danshen Tablets, DANQI PIAN etc., because not through purifying and making with extra care, active constituent content is lower, and not too clear and definite, drug action is not remarkable; Injection such as compound injection of red sage root, impurity is many, and active constituent content is too low, has clinically larger potential safety hazard, and its application has been subject to certain restriction.
The Chinese medicine cape jasmine is the dry mature fruit of madder wort cape jasmine Gardenia jasminoodes Ellis. All put down in writing cape jasmine in Chinese Pharmacopoeia and the many Chinese medicine books and have the purging intense heat relieving restlessness, reducing fever and causing diuresis, the effect of removing pattogenic heat from the blood and toxic material from the body, it is vexed to can be used for pyreticosis, and jaundice urine is red, blood strangury and dry pain, blood-head is told nosebleed, red eye, swell pain, pathogenic fire,toxin and furuncles etc., but also external curing bruise pain etc.
Summary of the invention
Purpose of the present invention just provides a kind for the treatment of cardiovascular and cerebrovascular diseases activity of having, and active ingredient is clear and definite, the Chinese medicine capejasmine extract that side effect is low.
Another object of the present invention provides a kind of preparation method of above-mentioned capejasmine extract.
A further object of the invention provides the application of above-mentioned capejasmine extract in the medicine of preparation treatment cardiovascular and cerebrovascular diseases.
The technical solution adopted for the present invention to solve the technical problems is: a kind of capejasmine extract, it is the extract that contains iridoid glycoside that extracts from the Chinese medicine cape jasmine, wherein contains the Gardenoside of weight percentage more than 30%.
Except containing Gardenoside, also contain Gardenoside and geniposide etc. in the above-mentioned capejasmine extract.
Determination of Gardenoside is more preferably more than 80% preferably more than 50% in the described capejasmine extract, take more than 90% as best.
The preparation method of above-mentioned capejasmine extract comprises the steps:
(1) preparation cape jasmine crude extract: get cape jasmine or pulverize after cape jasmine, the ethanol that adds water or 1%-95% extracts, and gets extract, and this extract is condensed into rare medicinal extract, namely gets the cape jasmine crude extract;
(2) refining: that the cape jasmine crude extract that described (1) step makes is crossed macroporous absorbent resin, the low-concentration ethanol wash-out of elder generation's water or 1%-30%, the eluent of this water or low-concentration ethanol is discarded need not, remove the impurity that is dissolved in polar solvent, use again the higher concentration ethanol elution of 40%-95%, collect this higher concentration ethanol eluate, higher concentration ethanol eluate behind the Recycled ethanol is dry, namely get the capejasmine extract that contains Gardenoside, namely get the Chinese medical extract with treatment cardiovascular and cerebrovascular diseases activity.
Wherein, water extracts the cape jasmine crude extract of preparation in (1) described above step, carrying out before described (2) went on foot macroporous absorbent resin, can further be condensed into relative density is the thick medicinal extract of 1.05-1.35, adding ethanol to concentration of alcohol again in described thick medicinal extract is 40-95%, leave standstill, get supernatant liquor and be condensed into rare medicinal extract as the cape jasmine crude extract.
If necessary, through the capejasmine extract that contains Gardenoside that described (2) one-step refining makes, available n-butanol or ethyl acetate or be further purified processing by silicagel column or alumina column chromatography.
Macroporous absorbent resin described in wherein said (2) one-step refining be in the macroporous absorbent resin of low polarity, as such as D101, D201, D301, AB-8, X-5 etc.
Drying means described in wherein said (2) step can be low temperature drying or drying under reduced pressure or spray-drying or freeze drying etc.
The application of above-mentioned capejasmine extract in the medicine of preparation treatment cardiovascular and cerebrovascular diseases contains the above-mentioned capejasmine extract of effective dose in the medicine of described treatment cardiovascular and cerebrovascular diseases.
The medicine of described treatment cardiovascular and cerebrovascular diseases, its formulation can be any existing pharmaceutical dosage forms in parenteral solution, transfusion, powder pin, dripping pill, tablet, sustained release tablets, capsule, soft capsule, the granule.
Described cardiovascular and cerebrovascular diseases comprise: any one or more illness in cerebral thrombus, cerebral ischemia, coronary heart diseases and angina pectoris, myocardial ischemia, heart failure, the arrhythmia cordis etc.
Compared with prior art, the invention has the beneficial effects as follows: prove that through pharmacodynamics test this capejasmine extract has the effect for the treatment of preferably cardiovascular and cerebrovascular diseases, side effect is less; Its active ingredient is clear and definite, i.e. contained iridoid glycoside constituents wherein, it mainly is Gardenoside, and the iridoid glycoside content take Gardenoside as representative in the extract is higher, other impurity components are then fewer, can reduce dose, also can reduce toxic and side effect to a certain extent, more be conducive to guarantee security and the validity of medicine.
The present invention follows the trail of the active component of cape jasmine, capejasmine extract with different Determination of Gardenosides is tested as medicine, and the result has confirmed the active ingredient of wherein the iridoid glycoside take Gardenoside as representative treatment cardiovascular and cerebrovascular diseases in the capejasmine extract. Active component screening and the curative effect of medicine of the present invention are proved by following pharmacodynamics test:
The test one: on senile rat in the thrombotic impact of body
Principle: use direct current continued stimulus arteria carotis communis 7 minutes, cause the endangium damage, activate blood platelet and blood coagulation system, vascular endothelial cell injury makes PGI simultaneously2Synthetic and discharge and reduce, cause and form gradually mixed thrombus in the carotid artery vascular. When carotid artery vascular internal cause thrombosis and during plug flow, blood vessel far-end temperature bust then. With temperature sensor monitors blood vessel surface variations in temperature, by the instrument automatic alarm, record begins to temperature bust required time from stimulation, claims duration of congestion OT, i.e. TFT. Time is shorter, represents easier formation thrombus; Otherwise the time is longer, represents more difficult formation thrombus.
But senile rat self-assembling formation blood stasis physique easily forms thrombus in vivo. Young rat then is difficult for forming thrombus. So the test in the positive contrast of senile rat, with the negative contrast of young rat.
Material: male rat. Young group mouse 3-4 in the age month is about body weight 250g. Old group mouse 24-27 in the age month, body is given birth to about 500g. Equipment: rat operation platform, operating scissors, ophthalmic tweezers, haemostatic clamp, mosquito clamp, rat oral gavage syringe needle, instrument for detecting internal thrombosis. Medicine and reagent: capejasmine extract (containing respectively Gardenoside is 0,30%, 50%, 80%, 90%) all is mixed with 50mg/ml; 20mg/ml amobarbital sodium solution; Physiological saline.
Method: experimental group is only given old group rat oral gavage 2ml/ with the 50mg/ml medicine every day, and positive controls senile rat and negative control group young rat gavage distilled water 2ml/, continuous 14 days. Drug withdrawal fasting on the same day. Lumbar injection 20mg/ml yellow Jackets 0.2ml/100g next day (body weight). Cut skin of neck, separate right carotid artery, transfer stimulating electrode at the arteria carotis near-end, far-end is transferred the temperature gauge head that connects instrument. Open instrument switch, give 1.5mV galvanic current stimulation 7 minutes with damage arteria carotis endothelial cell by stimulating electrode, along with thrombus in the arteria carotis tube chamber forms gradually, blood flow is blocked gradually, and the temperature of arteria carotis far-end descends gradually. When blood flow is blocked fully, the temperature bust, instrument is reported to the police, and shows duration of congestion OT, and the OT time is shorter, easier formation thrombus; The OT time is longer, more difficult formation thrombus.
Experimental result is carried out statistical test. Concrete numerical value and the results are shown in Table 1.
Table 1: on senile rat in the thrombotic impact of body
Medicine example number duration of congestion OT (min)
Capejasmine extract (containing Gardenoside is 0) 10 11.54 ± 1.78
Capejasmine extract (containing Gardenoside is 30%) 12 15.58 ± 1.64**
Capejasmine extract (containing Gardenoside is 50%) 11 16.99 ± 1.83***
Capejasmine extract (containing Gardenoside is 80%) 12 18.02 ± 1.58***
Capejasmine extract (containing Gardenoside is 90%) 12 18.38 ± 1.72***
Old positive controls 12 10.31 ± 1.28▲▲▲
Young negative control group 12 18.44 ± 1.20
Annotate:**P＜0.05
***Compare with the senile rat group P＜0.01.▲▲▲Compare with the young rat group P＜0.01.
By table 1 result of the test as can be known, senile rat OT is obviously short than young rat, illustrates easily to form thrombus. The capejasmine extract that does not contain Gardenoside almost can not make OT prolong. Along with the raising of Determination of Gardenoside in the capejasmine extract, the OT significant prolongation, Determination of Gardenoside is higher, and OT prolongs more obvious.
Above result shows that the capejasmine extract that contains Gardenoside has obvious anti-thrombosis function, and confirmation is the active ingredient in the cape jasmine take Gardenoside as main iridoid glycoside.
Test two: rat " rabbit brain powder-macromolecule glucan " is caused the therapeutic action of cerebral infarction
Principle: because cardiovascular and cerebrovascular disease all can cause hemorheological change, so can design capejasmine extract causes the therapeutic action of cerebral infarction to rat " rabbit brain powder-macromolecule glucan " pharmacodynamics test, investigate the change of hemorheological property behind the cerebral infarction to measure WBV under the different shear rates, investigate erythrocytic deformability with red blood cell albumen ringer solution viscosity, thereby investigate capejasmine extract to the therapeutic action of cardiovascular and cerebrovascular disease.
Material: animal: rat, body weight 250-350g, male and female are regardless of. Equipment: cone and plate viscometer (domestic NZ-6 type), centrifuge, scale centrifuge tube, eye scissors, ophthalmic tweezers and operating theater instruments commonly used, 0 trumpeter's art silk thread, blood vessel clip etc. Medicine and reagent: capejasmine extract (containing respectively Gardenoside is 0,30%, 50%, 80%, 90%); With the positive medicine contrast of commercially available danshen injections; Rabbit brain powder (rabbit brain powder APTT powder), the biochemical reagents experiment of Shanghai section is produced. Get the rabbit brain powder between the sub-sieve 120-150 order, particle is 100-120 μ m. Macromolecule glucan: molecular weight 5,000,000. The preparation of suppository: the 25mg rabbit brain powder is mixed among the 10% macromolecule dextran solution 100ml, places 37 ℃ of water-baths 40 minutes. Then, it is for subsequent use to be put in-18 ℃ of refrigerators. Rapid Medical ZT glue (Xi'an Research Inst. of Chemical Industry's production). BSA, ringer solution. Liquaemin: press 20u/ml blood dosage and add test tube, 40 ℃ of following dry for standby.
Test method: 1, the rat cerebral infarction model prepares: the rat etherization, and it is fixing to lie on the back, skin cropping sterilization, neck cuts, and neck always beats one's brains on the left of separating, neck is interior, external carotid artery. Folder closes external carotid artery, arteria carotis communis proximal part respectively. Press from both sides again a blood vessel clip at the distal end place. After suppository shaken up, lunge arteria carotis communis with the 0.25ml syringe by 0.03ml/100g rat dosage, open the distal end blood vessel clip, suppository is injected. Then, folder closes the arteria carotis communis distal end, extracts syringe needle, with the bonding pin hole of medical adhesive. Decontrol successively the blood vessel clip of arteria carotis communis distal end, proximal part, external carotid artery after 1 minute, recover blood flow, cleaning wound, skin suture.
Capejasmine extract on cerebral infarction after the Hemorheology impact of different time: rat is divided into 2 hours groups, 3 days groups, organized in 9 days, and every group is further divided into administration group (capejasmine extract+animal model group), physiological saline group (physiological saline+animal model group), sham-operation group (control group). Administration group, physiological saline group all impose operation technique as stated above, and sham-operation group operation technique is identical, but not injected plug agent with the physiologic saline for substitute suppository, is injected in internal carotid.
The administration group is in front 1 hour intraperitoneal injection of drugs (capejasmine extract, positive drug) 1.0mg/Kg of operation. The injection of physiological saline group is with amount physiological saline. The sham-operation group is not injected any medicine. Every morning administration 1 time after 3 days groups and the 9 days groups, for three days on end or 9 days.
2 hours after surgery, the 3rd day, the 9th day respectively, with rat anesthesia (25% urethane 0.3ml/100g body weight, lumbar injection), the RCCA bloodletting was measured WBV under the different shear rates with cone and plate viscometer in 2 hours in the heparin test tube. Again that whole blood is centrifugal with 1500rpm, suck upper plasma. Then use 0.25% bovine serum albumin(BSA)-ringer solution rinsing red blood cell three times, centrifugal 10 minutes of each 1500rpm. At last, in vitro be mixed with red blood cell at scale: albumen is appointed the red blood cell albumen ringer solution of liquid=6: 4, measures its viscosity at 20 seconds under-1 shear rate. With red blood cell albumen ringer solution viscosity as ED. All experiments are all carried out under 25 ℃ of constant temperature, and experimental result is carried out statistical test. Concrete numerical value and the results are shown in Table 2, table 3.
Table 2: capejasmine extract (injection) is on the WBV impact (unit: mPa.s) of different time behind the rat cerebral infarction
| Cape jasmine cuts the thing rate that becomes of extracting | 2h | 3d | 9d |
| Physiology salt administration group control group water group | Physiology salt administration group control group water group | Physiology salt administration group control group water group | |
| Contain Cape jasmine 100s-1Sub-glycosides 20s-1 0％ 10s -1 | 7.79±0.2 7.64±0.8 7.57±0.8 10.15±1.4 9.97±1.1 8.35±1.0*** 10.89±0.7 9.68±1.3** 9.04±0.8*** 12.51±3.2 11.89±2.2 11.05±1.5 17.17±2.3 15.75±2.3 14.20±2.5** 20.31±2.5 18.89±3.2** 15.39±2.1*** 41.26±18.2 37.31±7.4 33.89±14.5 82.81±21.3 75.23±14.7 49.73±21.5** 93.99±20.9 85.81±25.3 55.25±12.1*** | ||
| Contain Cape jasmine 100s-1Sub-glycosides 20s-1 30％ 10s -1 | 7.79±0.2 7.21±0.3 7.57±0.8 10.15±14 8.44±0.3 *** 8.35±1.0 *** 10.89±0.7 8.51±1.2 *** 9.04±0.8 *** 12.51±3.2 11.22±2.3 11.05±1.5 17.17±2.3 15.21±4.3 ** 14.20±2.5 ** 20.31±2.5 16.73±3.1 ** 15.39±2.1 *** 41.26±18.2 34.31±8.4 33.89±14.5 82.81±21.3 62.58±17.1 ** 49.73±21.5 ** 93.99±20.9 58.82±21.3 ** 55.25±12.1 *** | ||
| Contain Cape jasmine 100s-1Sub-glycosides 20s-1 50％ 10s -1 | 7.79±0.2 7.11±0.8 7.57±0.8 10.15±1.4 8.31±0.6 *** 8.35±1.0 *** 10.89±0.7 8.43±1.1 *** 9.04±0.8 *** 12.51±3.2 10.74±2.1 11.05±1.5 17.17±2.3 14.55±2.2 ** 14.20±2.5 ** 20.31±2.5 14.07±3.2 *** 15.39±2.1 *** 41.26±18.2 31.98±8.4 33.89±14.5 82.81±21.3 54.71±15.5 ** 49.73±21.5 ** 93.99±20.9 54.91±24.8 *** 55.25±12.1 *** | ||
| Contain Cape jasmine 100s-1Sub-glycosides 20s-1 80％ 10s -1 | 7.79±0.2 7.06±0.5 7.57±0.8 10.15±1.4 8.17±1.1 *** 8.35±1.0 *** 10.89±0.7 8.31±0.7 *** 9.04±0.8 *** 12.51±3.2 10.32±2.3 11.05±1.5 17.17±2.3 12.21±2.1 ** 14.20±2.5 ** 20.31±2.5 13.33±2.4 *** 15.39±2.1 *** 41.26±18.2 31.78±81 33.89±14.5 82.81±21.3 49.31±11.1 ** 49.73±21.5 ** 93.99±20.9 51.42±173 *** 55.25±12.1 *** | ||
| Contain Cape jasmine 100s-1Sub-glycosides 20s-1 90％ 10s -1 | 7.79±0.2 7.02±0.5 7.57±0.8 10.15±1.4 8.02±0.7 *** 8.35±1.0 *** 10.89±0.7 8.09±0.6 *** 9.04±0.8 *** 12.51±3.2 10.13±2.1 11.05±1.5 17.17±2.3 13.98±1.7 *** 14.20±2.5 ** 20.31±2.5 12.21±3.2 *** 15.39±2.1 *** 41.26±18.2 30.84±8.1 33.89±14.5 82.81±21.3 48.43±13.1 *** 49.73±21.5 ** 93.99±20.9 47.23±21.6 *** 55.25±12.1 *** | ||
| Red sage root 100s-1Injection 20s-1Liquid 10s-1 | 7.79±0.2 7.42±0.7 7.57±0.8 10.15±1.4 9.43±1.1 8.35±1.0 ** 10.89±0.7 9.87±0.7 ** 9.04±0.8 *** 12.51±3.2 11.54±2.3 11.05±1.5 17.17±2.3 16.86±2.1 14.20±2.5 ** 20.31±2.5 18.87±4.0 ** 15.39±2.1 *** 41.26±18.2 36.66±14.9 33.89±14.5 82.81±21.3 74.40±13.8 49.73±21.5 ** 93.99±20.9 84.21±20.7 55.25±12.1 *** |
| Annotate: all compare with the physiological saline group * * P＜0.05 * * * P＜0.01. | |
Table 3: capejasmine extract (injection) is on the impact (unit: mPa.s) of different time red blood cell-albumen ringer solution viscosity
| Capejasmine extract | 2h | 3d | 9d |
| Physiological saline group administration group control group | Physiological saline group administration group control group | Physiological saline group administration group control group | |
| Contain Gardenoside 0% | 4.93±0.2 4.83±0.2 4.52±0.3 5.14±0.4 5.12±0.7 4.22±0.5 *** 5.22±0.4 5.15±0.5 4.19±0.4 *** | ||
| Contain Gardenoside 30% | 4.93±0.2 4.68±0.5 4.52±0.3 5.14±0.4 4.44±0.5 ** 4.22±0.5 *** 5.22±0.4 4.35±0.5 *** 4.19±0.4 *** | ||
| Contain Gardenoside 50% | 4.93±0.2 4.64±0.4 4.52±0.3 5.14±0.4 4.31±0.4 *** 4.22±0.5 *** 5.22±0.4 4.21±0.3 *** 4.19±0.4 *** | ||
| Contain Gardenoside 80% | 4.93±0.2 4.67±0.5 4.52±0.3 5.14±0.4 425±0.6 *** 4.22±0.5 *** 5.22±0.4 4.12±0.4 *** 4.19±0.4 *** | ||
| Contain Gardenoside 90% | 4.93±0.2 4.32±0.4 4.52±0.3 5.14±0.4 4.17±0.5 *** 4.22±0.5 *** 5.22±0.4 4.08±0.3 *** 4.19±0.4 *** | ||
| Danshen injections | 4.93±0.2 4.75±0.5 4.52±0.3 5.14±0.4 4.54±0.6 ** 4.22±0.5 *** 5.22±0.4 4.34±0.6 *** 4.19±0.4 *** | ||
| Annotate: all compare with the physiological saline group * * P＜0.05 * * * P＜0.01. | |||
By table 2 result of the test as can be known, block rear 2 hours after, WBV is respectively organized equal no significant difference. When blocking 3 days, the physiological saline group is compared with the sham-operation group, WBV rising (P＜0.05), animal model modeling success is described, each administration group all can reduce WBV to some extent, along with the raising of Determination of Gardenoside in the capejasmine extract, effect become better and better (P＜0.01). When blocking after 9 days, the physiological saline group is abnormality still with sham-operation group ratio, Hemorheology, and WBV further increases the weight of. Each administration group and physiological saline group ratio, WBV descend, and statistical procedures has significant, and along with the raising of Determination of Gardenoside in the capejasmine extract, effect is become better and better, and effect is better than danshen injections.
By table 3 result of the test as can be known, block rear 2 hours after, physiological saline group and administration group ED descend, each administration group is slightly lower than physiological saline group numerical value, but effect is very unobvious. When blocking 3 days, the physiological saline group is compared with the sham-operation group, and ED further descends, and except the capejasmine extract that does not contain Gardenoside, all can stop to a certain extent ED to descend in all the other each administration groups. When blocking after 9 days, physiological saline group and sham-operation group ratio, ED further descends. Except the capejasmine extract that does not contain Gardenoside, each administration group and physiological saline group ratio, all can improve and stop the decline of ED, statistical procedures has significant (P＜0.01), and along with the raising of Determination of Gardenoside in the capejasmine extract, effect become better and better (P＜0.01). And be better than danshen injections.
In sum, perform the operation after 2 hours, rat is existing hemorheological unusual. Blocked 3-9 days, Abnormal Blood Rheology further increases the weight of, and shows as WBV and raises degradation under the ED. The capejasmine extract that contains Gardenoside can play and improve hemorheological property effect behind the cerebral infarction, and along with the raising of Determination of Gardenoside in the capejasmine extract, effect is become better and better. After the 3rd day, then can correct significantly unusual Hemorheology and change. And successful is better than danshen injections. Test has confirmed that the iridoid glycoside take Gardenoside as the master is the active ingredient in the cape jasmine.
The specific embodiment
The present invention is described in further detail below in conjunction with the specific embodiment.
Embodiment one
Get cape jasmine 100kg, add water 800kg, boil and extracted 1 hour, filter, filtrate for later use, the dregs of a decoction add water 700kg again, boil and extracted 1 hour, filter, merge filtrate twice, it is rare medicinal extract of 1.08 that filtrate after merging is condensed into relative density, this rare medicinal extract is crossed the D101 macroporous absorbent resin, wash with water first to colourless, this water elution liquid is discarded, use again 85% ethanol elution to colourless, collect this 85% ethanol eluate, it is 1.11 thick medicinal extract that 85% ethanol eluate behind the Recycled ethanol is condensed into relative density, with this thick medicinal extract spray-drying, obtain containing the capejasmine extract of Gardenoside 50%, namely get Determination of Gardenoside and be 50% the Chinese medical extract with the effect for the treatment of cardiovascular and cerebrovascular diseases.
Embodiment two
Get cape jasmine 100kg, add water 900kg, boil and extracted 2 hours, filter filtrate for later use, the dregs of a decoction add water 900kg again, boil and extracted 1 hour, filter, merge filtrate twice, be concentrated into relative density 1.05, adding ethanol to ethanol content is 40%, leaves standstill 18 hours, gets supernatant liquor, it is rare medicinal extract of 1.02 that this supernatant liquor Recycled ethanol is become relative density, this rare medicinal extract is crossed the D201 macroporous absorbent resin, use first 15% ethanol elution to colourless, this 15% ethanol eluate is discarded, use again 60% ethanol elution to colourless, collect this 60% ethanol eluate, it is 1.10 thick medicinal extract that 60% ethanol eluate behind the Recycled ethanol is condensed into relative density, with this thick medicinal extract drying under reduced pressure, obtain containing the capejasmine extract of Gardenoside 40%, namely get Determination of Gardenoside and be 40% the Chinese medical extract with the effect for the treatment of cardiovascular and cerebrovascular diseases. In this Determination of Gardenoside is 40% capejasmine extract, the water that adds 5 times of amounts, heating makes dissolving, add again extracting n-butyl alcohol 3 times, each n-butanol consumption equates with the water yield, and combining extraction liquid is with dry behind the extract recovery n-butanol after merging, can contain Gardenoside and be 90% capejasmine extract, namely get Determination of Gardenoside and be 90% the Chinese medical extract with the effect for the treatment of cardiovascular and cerebrovascular diseases.
Embodiment three
Get cape jasmine 100kg, add water 1000kg, boil and extracted 2 hours, filter filtrate for later use, the dregs of a decoction add water 900kg again, boil and extracted 1 hour, filter filtrate for later use, the dregs of a decoction add water 900kg again, boil and extracted 1 hour, filter, merge three times filtrate, be concentrated into relative density 1.05, adding ethanol to ethanol content is 95%, leaves standstill 24 hours, gets supernatant liquor, it is rare medicinal extract of 1.05 that this supernatant liquor Recycled ethanol is become relative density, this rare medicinal extract is crossed the D201 macroporous absorbent resin, use first 20% ethanol elution to colourless, this 20% ethanol eluate is discarded, use again 50% ethanol elution to colourless, collect this 50% ethanol eluate, it is 1.09 thick medicinal extract that 50% ethanol eluate behind the Recycled ethanol is condensed into relative density, with this thick medicinal extract drying under reduced pressure, obtain containing the capejasmine extract of Gardenoside 60%, namely get Determination of Gardenoside and be 60% the Chinese medical extract with the effect for the treatment of cardiovascular and cerebrovascular diseases.
Embodiment four
Get cape jasmine 100kg, add 1% ethanol 700kg, refluxing extraction 1.5 hours, filter, filtrate for later use, the dregs of a decoction add 1% ethanol 700kg again, refluxing extraction 1.5 hours filters, and merges filtrate twice, it is rare medicinal extract of 1.05 that filtrate after merging is concentrated in relative density, this rare medicinal extract is crossed the AB-8 macroporous absorbent resin, use first 10% ethanol elution to colourless, this 10% ethanol eluate is discarded, use again 70% ethanol elution to colourless, collect this 70% ethanol eluate, it is 1.10 thick medicinal extract that 70% ethanol eluate behind the Recycled ethanol is condensed into relative density, with this thick medicinal extract spray-drying, obtain containing the capejasmine extract of Gardenoside 30%, namely get Determination of Gardenoside and be 30% the Chinese medical extract with the effect for the treatment of cardiovascular and cerebrovascular diseases. In this Determination of Gardenoside is 30% capejasmine extract, the ethanol that adds 0.5 times, heating makes dissolving, by alumina column (the aluminium oxide consumption is 10 times of extract consumption), with ethyl acetate-acetone-water (5: 5: 2) wash-out, collect the component that contains Gardenoside again, reclaim solvent, drying obtains containing Gardenoside and is 95% capejasmine extract, namely gets Determination of Gardenoside and be 95% the Chinese medical extract with the effect for the treatment of cardiovascular and cerebrovascular diseases.
Embodiment five
Get cape jasmine 100kg, add 95% ethanol 800kg, refluxing extraction 1.5 hours, filter, filtrate recycling ethanol to nothing alcohol is distinguished the flavor of, it is rare medicinal extract of 1.06 that thin up becomes relative density, this rare medicinal extract is crossed the D301 macroporous absorbent resin, use first 30% ethanol elution to colourless, this 30% ethanol eluate is discarded, use again 95% ethanol elution to colourless, collect this 95% ethanol eluate, it is 1.35 thick medicinal extract that 95% ethanol eluate behind the Recycled ethanol is condensed into relative density, with this thick medicinal extract oven dry, obtain containing the capejasmine extract of Gardenoside 80%, namely get Determination of Gardenoside and be 80% the Chinese medical extract with the effect for the treatment of cardiovascular and cerebrovascular diseases.
Embodiment six
Get cape jasmine 100kg, add 50% ethanol 700kg, refluxing extraction 1.5 hours, filter, filtrate for later use, the dregs of a decoction add 50% ethanol 700kg again, refluxing extraction 1.5 hours filters, and merges filtrate twice, it is rare medicinal extract of 1.08 that filtrate recycling ethanol after merging is become relative density, this rare medicinal extract is crossed the X-5 macroporous absorbent resin, use first 1% ethanol elution to colourless, this 1% ethanol eluate is discarded, use again 40% ethanol elution to colourless, collect this 40% ethanol eluate, it is 1.13 thick medicinal extract that 40% ethanol eluate behind the Recycled ethanol is condensed into relative density, with this thick medicinal extract spray-drying, obtain containing the capejasmine extract of Gardenoside 35%, namely get Determination of Gardenoside and be 35% the Chinese medical extract with the effect for the treatment of cardiovascular and cerebrovascular diseases. In this Determination of Gardenoside is 35% capejasmine extract, the water that adds 5 times of amounts, heating makes dissolving, add again ethyl acetate extraction 3 times, each ethyl acetate consumption equates with the water yield, and combining extraction liquid is with dry behind the extract recovery of acetic acid ethyl ester after merging, obtain containing Gardenoside and be 70% capejasmine extract, namely get Determination of Gardenoside and be 70% the Chinese medical extract with the effect for the treatment of cardiovascular and cerebrovascular diseases.
Embodiment seven
Get the described capejasmine extract 3kg that contains Gardenoside, vegetable oil 7kg, mixing is made capsule casing material with gelatin, is pressed into soft capsule, namely makes the pharmaceutical composition of the soft capsule dosage form that contains 30% capejasmine extract.
Embodiment nine
Get the described capejasmine extract 300g that contains Gardenoside, be dissolved in the 10000ml water for injection, adopt existing powder-injection freeze-drying preparation technology, namely make the pharmaceutical composition of the powder-injection type that contains capejasmine extract.
Embodiment ten
Get the described capejasmine extract 300g that contains Gardenoside, starch 700g mixes, and adopts existing capsules preparation technique, namely makes the pharmaceutical composition of the capsule formulation that contains capejasmine extract.
Embodiment 11
Get the described capejasmine extract 300g that contains Gardenoside, adopt dripping pill preparation technology, namely make the pharmaceutical composition of the drops that contains capejasmine extract.
Embodiment 12
Get the described capejasmine extract 300g that contains Gardenoside, sucrose 800g mixes, and granulates, and sieves, and drying namely makes the pharmaceutical composition of the particle formulation that contains capejasmine extract; Maybe with the particle that makes through further compressing tablet, drying namely makes the pharmaceutical composition of the Tabules that contains capejasmine extract.
Embodiment 13
Get the described capejasmine extract 300g that contains Gardenoside, polyethylene 60g mixes, granulate, and compressing tablet, drying namely makes the pharmaceutical composition of the sustained release tablets formulation that contains capejasmine extract.
Embodiment 14
Get the described capejasmine extract 50g that contains Gardenoside, be dissolved in the 10000ml water for injection, adopt process for preparation of injection, namely make the parenteral solution (containing transfusion) of 5mg/ml.
Embodiment 15
Get the described capejasmine extract 300g that contains Gardenoside, other gets ginsenoside 100g, and sucrose 600g mixes, and granulates, sieve, and drying, compressing tablet namely makes the pharmaceutical composition of the Tabules that contains capejasmine extract and ginsenoside.
Claims (10)
1, a kind of capejasmine extract, it is the extract that contains iridoid glycoside of the preparation take the Chinese medicine cape jasmine as raw material, it is characterized in that: contain the Gardenoside of weight percentage more than 30% in the described capejasmine extract.
2, capejasmine extract according to claim 1 is characterized in that: contain the Gardenoside of weight percentage more than 50% in the described capejasmine extract.
3, capejasmine extract according to claim 1 is characterized in that: contain the Gardenoside of weight percentage more than 80% in the described capejasmine extract.
4, a kind of preparation method of capejasmine extract claimed in claim 1 may further comprise the steps:
(1) preparation cape jasmine crude extract: get cape jasmine or pulverize after cape jasmine, the ethanol that adds water or 1%-95% extracts, and gets extract, and this extract is condensed into rare medicinal extract, namely gets the cape jasmine crude extract;
(2) refining: that the cape jasmine crude extract that described (1) step makes is crossed macroporous absorbent resin, the low-concentration ethanol wash-out of elder generation's water or 1%-30%, the eluent of this water or low-concentration ethanol is discarded need not, use again the higher concentration ethanol elution of 40%-95%, collect this higher concentration ethanol eluate, higher concentration ethanol eluate behind the Recycled ethanol is dry, namely get the capejasmine extract that contains Gardenoside.
5, the preparation method of capejasmine extract according to claim 4, it is characterized in that: water extracts the cape jasmine crude extract of preparation in described (1) step, carrying out before described (2) went on foot macroporous absorbent resin, can further be condensed into relative density is the thick medicinal extract of 1.05-1.35, adding ethanol to concentration of alcohol again in described thick medicinal extract is 40-95%, leave standstill, get supernatant liquor and be condensed into rare medicinal extract as the cape jasmine crude extract.
6, according to claim 4 or the preparation method of 5 described capejasmine extracts, it is characterized in that: through the capejasmine extract that contains Gardenoside of described (2) one-step refining gained, available extracting n-butyl alcohol or ethyl acetate extraction or silica gel column chromatography or alumina column chromatography are further purified processing.
7, according to claim 4 or the preparation method of 5 described capejasmine extracts, it is characterized in that: the macroporous absorbent resin described in described (2) one-step refining be in the macroporous absorbent resin of low polarity.
8, a kind of claim 1 or the 2 or 3 described capejasmine extracts application in the medicine of preparation treatment cardiovascular and cerebrovascular diseases is characterized in that: the described capejasmine extract that contains effective dose in the medicine of described treatment cardiovascular and cerebrovascular diseases.
9, the application of capejasmine extract according to claim 8 in the medicine of preparation treatment treatment cardiovascular and cerebrovascular diseases, it is characterized in that: the formulation of described medicine can be any existing pharmaceutical dosage form in parenteral solution, transfusion, powder pin, dripping pill, tablet, sustained release tablets, capsule, soft capsule, the granule.
10, the application of capejasmine extract according to claim 8 in the medicine of preparation treatment treatment cardiovascular and cerebrovascular diseases, it is characterized in that: described cardiovascular and cerebrovascular diseases comprise: any one or more illness in cerebral thrombus, cerebral ischemia, coronary heart diseases and angina pectoris, myocardial ischemia, heart failure, the arrhythmia cordis.
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| CN1307192C (en) * | 2005-05-24 | 2007-03-28 | 中国人民解放军第二军医大学 | Process of preparing high-purity jasminodin with Cape jasmine fruit |
| CN1307193C (en) * | 2005-05-24 | 2007-03-28 | 中国人民解放军第二军医大学 | Process of preparing total iridoid glycoside with cape jasmine fruit |
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Assignee: Sichuan Hebang Sunlight Pharmaceutical Co., Ltd. Assignor: Li Wenjun Contract fulfillment period: 2009.1.15 to 2015.1.15 contract change Contract record no.: 2009510000054 Denomination of invention: Cape jasmine extract , its preparing process and application Granted publication date: 20081231 License type: Exclusive license Record date: 2009.9.21 |
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