CN1562097A - Fructus choerospondiatis freeze-drying powder injection and its preparing method - Google Patents
Fructus choerospondiatis freeze-drying powder injection and its preparing method Download PDFInfo
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Abstract
A freeze dried powder injection of choerospondias fruit for treating cardiovascular disease is prepared through extracting active component from choerspondias fruit in alcohol, purifying, proportionally mixing it with medicinal auxiliaries and freeze drying.
Description
Affiliated technical field
The invention belongs to field of traditional Chinese medicine pharmacy, be specifically related to a kind of Fructus Choerospondiatis lyophilized injectable powder and preparation method thereof.
Background technology
Cardiovascular disease is various because of its pathogenic factors, the pathomechanism complexity, how because of weakness due to chronic disease, excessive thinking and anxiety damage motive heart-yang institute extremely, treat very thornyly, and be called one of human main causes of death by modern medicine.Cardiopalmus is conscious nervous uneasiness, can not be autonomous, or the uneven a kind of syndrome of pulse condition, clinically be more common in heart disease, angina pectoris, and be coronary insufficiency, temporary transient ischemia and the caused clinical syndrome of anoxia that cardiac muscle is rapid.The cardiopathic medicine of research treatment has a lot, as nitroglycerin, is characterized in that onset is rapid, but has certain toxic and side effects; Also have some Chinese patent medicines, FUFANG DANSHEN ZHUSHEYE for example, the alginate diester sodium injection, MAILUONING ZHUSHEYE etc., though to heart disease, coronary heart disease, angina pectoriss etc. have curative effect preferably, changed the slow deficiency of solid preparation onset, but the report of its untoward reaction also increases year by year, report that wherein FUFANG DANSHEN ZHUSHEYE has anaphylaxis 58 examples, drug eruption 23 examples, totally 131 routine untoward reaction such as dead 2 examples, the alginate diester sodium injection has anaphylaxis 31 examples, leukopenia 25 examples, gastrointestinal reaction 23 examples, totally 128 routine untoward reaction such as dead 1 example, MAILUONING ZHUSHEYE has anaphylaxis 28 examples, totally 68 routine untoward reaction such as anaphylactic shock 18 examples.Although cause that the factor of untoward reaction is more, mechanism is unclear fully yet, and clinical exigence medicine is safely and effectively determined.
Fructus Choerospondiatis is the dry mature fruit of Anacardiaceae plant Fructus Choerospondiatis Choerospondias axillaries (Roxb.) Burtt et Hill, is the medical material that promoting flow of QI and blood, tranquilizing by nourishing the heart are commonly used by the Mongols, uses very extensively in China Mongolian medicine medicine, and main product is in Guangdong.Fructus Choerospondiatis sweet in the mouth, acid, property is flat, greasy, heavy, gentle; The clearing away heart-fire promoting flow of QI and blood is arranged, nourish heart, mind-easing function.Be mainly used in qi depression to blood stasis, the thoracic obstruction is had a pain, shortness of breath and palpitation, diseases such as irritability.Modern pharmacology studies confirm that, the Fructus Choerospondiatis total flavones can obviously reduce wastage of grain, etc. caused by rats oxygen speed and oxygen consumption, improves hypoxia-bearing capability, coronary artery dilator; Improve hemorheological indexes, remove free radical, improve SOD in the heart tissue activity [bag is saved from damage etc. the experimentation of Fructus Choerospondiatis total flavones antioxidation.China's pharmacology and clinical.2001，17(2)：8]。The Fructus Choerospondiatis total flavones has obvious protective effect to myocardial ischemia; obviously dwindle myocardial infarct size; alleviate the treating myocardial ischemia damage degree; infer its mechanism of action may with regulate the various enzymatic activitys of body relevant [Tang Li etc. Fructus Choerospondiatis is studied the Acute Myocardial Ischemia in Rats protective effect. Chinese medicine journal .2003,31 (3): 50].The Fructus Choerospondiatis water soluble polysaccharide has the myocardium shrinkage function of improvement to anxious Terrier, dwindles myocardial infarction area, alleviates the effect of myocardial damage, and the rat heart muscle ischemia that pituitrin is caused has significant protective effect, can obviously resist BaCl
2Rat ventricular that brings out and CHCL
3Decreased heart rate is quivered in the mice chamber of bringing out.Fructus Choerospondiatis is widely used in Chinese medicine, and polygamy side uses as Fructus Choerospondiatis seven flavor balls, compound recipe Fructus Choerospondiatis injection etc. clinically; The patent that relates to the Fructus Choerospondiatis application in the Chinese patent is more, but the overwhelming majority is a compound solid preparation, there is not the medicine that relates to the Fructus Choerospondiatis ejection preparation, CN93110427 discloses extracting solution of Fructus Choerospondiatis and the solid preparation that the Fructus Choerospondiatis coarse powder is mixed and made into, still belong to a kind of more primary pharmaceutical preparation, though the research report of Fructus Choerospondiatis injection is arranged in the relevant report, not seeing has the clinical practice report, does not up to the present see the lyophilized injectable powder report that the Fructus Choerospondiatis effective ingredient is made as yet.
Summary of the invention
Based on above factor, after the method that the present invention adopts ethanol extraction, macroporous adsorbent resin method and ultrafiltration to organically combine is extracted purification to Fructus Choerospondiatis effective site, after excipient substance mixes, prepare the Chinese medicine powder injection through lyophilization, The pharmacological results shows, this lyophilized injectable powder has better curative effect to cardiovascular disease, compares with similar medicine, has stronger pharmacological action.
One. process recipes
Get Fructus Choerospondiatis, put into the Chinese medicine multi-function extractor, with 6-10 50%-80% ethanol extraction doubly, extract 2-4 time, each 1-3 hour, extracting solution merged, and reclaimed ethanol to the greatest extent, obtained not having pure clear paste, and standby, filter residue and drying is standby; Get no pure clear paste, drying, last HP type macroporous adsorptive resins is with the distilled water eluting of 8-12 times of column volume, eluent is standby, and reuse concentration 20%-80%, 6-8 times column volume ethanol elution is collected eluent, reclaim ethanol to the greatest extent, obtain the Fructus Choerospondiatis general flavone material, standby; Get dry filtering residue and water elution liquid and merge, put into the Chinese medicine multi-function extractor, add 6-8 times of water, extract 2-4 time, each 2-4 hour, merge extractive liquid,, being evaporated to relative density is 1.15-1.20 (50 ℃), adding ethanol makes alcoholic degree reach 50%-70% (V/V), staticly settle, filter, filtrate adds ethanol again makes determining alcohol reach 75%-90%, staticly settle, filter, merge precipitation, the precipitation dissolved in distilled water, make in the solution every milliliter to amount to raw medicinal herbs 1 gram, after the filtration, with the ultrafilter membrane ultrafiltration of molecular cut off 3000 3-5 time, at every turn during ultrafiltration 1/2-1/3, adding distil water is to original volume, concentrated solution, concentrated solution reuse molecular cut off is 100,000 ultrafilter membrane ultrafiltration 3-5 time, at every turn during ultrafiltration 1/2-1/3, adding distil water is to original volume, collect ultrafiltrate, vacuum concentration, making the solution pol is 2%-5%, obtain Fructus Choerospondiatis water soluble polysaccharide concentrated solution, standby.Get Fructus Choerospondiatis total flavones and freeze-dried excipient and be dissolved in the Fructus Choerospondiatis water soluble polysaccharide concentrated solution, filter, in the packing cillin bottle, be prepared into the Fructus Choerospondiatis freeze-dried powder by the requirement lyophilization of Chinese medicine lyophilized injectable powder with the 0.45um microporous filter membrane.
Two. pharmacology embodiment
Embodiment 1
Influence to isolated rat heart anoxia arrhythmia
Medicine: lyophilized injectable powder of the present invention (Qianluchun Science and Technology Co., Ltd., Beijing's laboratory provides)
Compound recipe Fructus Choerospondiatis injection (Inner Mongol Chinese medicine academy provides)
Normal saline (Qianluchun Science and Technology Co., Ltd., Beijing's laboratory provides)
Experimental technique: 24 of rats, body weight 256 ± 23g is divided into 3 groups at random.The preparation isolated heart is used the guiding of volume conduction method and observes and write down electrocardio to change, and stablizes 20 minutes.The anoxia matched group is used instead and is contained purity nitrogen K-H perfusate, and the administration group is observed 20 member record arrhythmia time of occurrences and asystole time continuously with freeze-dried powder remover liquid injection of the present invention, compound recipe Fructus Choerospondiatis injection, purity nitrogen K-H perfusate.
Lyophilized injectable powder of the present invention is to the influence of isolated rat heart anoxia arrhythmia: arrhythmia and asystole all appear in matched group 8 routine hearts.But lyophilized injectable powder of the present invention and compound recipe Fructus Choerospondiatis injection are obviously to the anti-hypoxia arrhythmia, and be good dose-effect relationship, but significant prolongation arrhythmia time of occurrence, obviously reduce incidence of arrhythmia, experimental result shows that also lyophilized injectable powder group of the present invention and compound recipe Fructus Choerospondiatis injection group relatively have significant difference.Experimental result sees Table 1:
Table 1 is respectively organized the influence of preparation to isolated rat heart anoxia arrhythmia
| Group | Arrhythmia time of occurrence (branch) | Incidence of arrhythmia (%) | The asystole time (branch) | Asystole rate (%) |
| Normal saline | ??11.01 | 100 | ??12.33 | ??100 |
| Compound recipe Fructus Choerospondiatis injection | ??14.02 ** | 33 | ??5.50 | ??50 |
| Lyophilized injectable powder of the present invention | ??17.13 **[ *] | 17 | ??- | ??- |
*P＜0.01; [
*] P＜0.05, processed group and positive controls are relatively.
Embodiment 2
To the Acute Myocardial Ischemia in Rats protective effect
Medicine: lyophilized injectable powder of the present invention (Qianluchun Science and Technology Co., Ltd., Beijing's laboratory provides)
FUFANG DANSHEN ZHUSHEYE (Shanghai first Bioceuticals Inc.)
Normal saline (Qianluchun Science and Technology Co., Ltd., Beijing's laboratory provides)
Materials and methods: 60 of animal Wister rat, male, body weight (300 ± 20) g is provided by Beijing University of Chinese Medicine's Experimental Animal Center.Rat is divided into 3 groups at random by body weight, 20 every group.Be divided into model group, compound Salviae Miltiorrhizae positive drug control group, lyophilized injectable powder group of the present invention.Each organizes equal intravenous injection, causes the acute myocardial ischemia model by the ramus descendens anterior arteriae coronariae sinistrae of literature method ligation rat.20% urethane (1g/kg, ip) anesthesia separates common carotid artery, and parallel trachea is inserted art, connects animal respirator.Left side the 4th intercostal is opened breast, cuts off pericardium, separates ramus descendens anterior arteriae coronariae sinistrae, and the ligation position is done in flat right auricle.The taking-up heart is weighed,-10 ℃ of freezing 30～50min, under the heart ligature, parallel coronary sulcus becomes 5 with the ventricle crosscut, behind the normal saline flushing, the concentration that places the preparation of pH value 8.0 phosphate buffers is 1% triphenyltetrazolium chloride (TTC) solution, 10min dyes in 38 ℃ of waters bath with thermostatic control, normal myocardium is coloured to kermesinus, infarcted myocardium is dyed lark, cuts off the part that myocardium sheet is colored, and the ischemic infarction district cardiac muscle that is not colored is weighed, (the ischemic infarction area accounts for heavy whole-heartedly percentage ratio, the results are shown in Table 2 to calculate the ischemia scope.
Table 2 is respectively organized preparation to the Acute Myocardial Ischemia in Rats protective effect
| Group | Heart heavy (g) | Heart infarction heavy (g) | Heart infarction percentage rate (%) |
| Normal saline | 0.985 | ?0.122 | ?12.34 |
| FUFANG DANSHEN ZHUSHEYE | 0.843 | ?0.087 | ?10.29 ** |
| Lyophilized injectable powder of the present invention | 0.865 | ?0.057 | ?6.64 **[ *] |
*P＜0.01; [
*] P＜0.05, processed group and positive controls are relatively.
Conclusion: above pharmacological evaluation shows that lyophilized injectable powder of the present invention has great pharmacological effects to cardiovascular disease, compares with similar drug, has better pharmacological effect.
Three. preparation embodiment
Embodiment 1
Get Fructus Choerospondiatis 1000 grams, put into the Chinese medicine multi-function extractor, with 6 times 50% ethanol extraction, extract 2 times, each 1 hour, extracting solution merged, and reclaimed ethanol to the greatest extent, obtained not having pure clear paste, and standby, filter residue and drying is standby; Get no pure clear paste, drying, last HP-10 type macroporous adsorptive resins, with the distilled water eluting of 8 times of column volumes, eluent is standby, and reuse concentration 20%, 6 times of column volume ethanol elutions are collected eluent, reclaim ethanol to the greatest extent, obtain Fructus Choerospondiatis total flavones 68.97 grams, and are standby; Get dry filtering residue and water elution liquid and merge, put into the Chinese medicine multi-function extractor, add 6 times of water, extract 2 times, each 2 hours, merge extractive liquid,, being evaporated to relative density is 1.15 (50 ℃), adds ethanol and makes alcoholic degree reach 50% (V/V), staticly settles, filter, filtrate adds ethanol again makes determining alcohol reach 75%, staticly settles, filter, merge precipitation, the precipitation dissolved in distilled water, make in the solution every milliliter to amount to raw medicinal herbs 1 gram, after the filtration, with the ultrafilter membrane ultrafiltration of molecular cut off 3,000 3 times, during each ultrafiltration to 1/2, adding distil water is to original volume, concentrated solution, concentrated solution reuse molecular cut off is 100,000 ultrafilter membrane ultrafiltration 3 times, during each ultrafiltration to 1/2, adding distil water is to original volume, collect ultrafiltrate, vacuum concentration, making the solution pol is 2%, obtain Fructus Choerospondiatis water soluble polysaccharide concentrated solution 172.41 grams, standby.Getting Fructus Choerospondiatis total flavones and freeze-dried excipient mannitol 7135.42 grams is dissolved in the Fructus Choerospondiatis water soluble polysaccharide concentrated solution, filter with the 0.45um microporous filter membrane, in the packing cillin bottle, be prepared into the Fructus Choerospondiatis freeze-dried powder by the requirement lyophilization of Chinese medicine lyophilized injectable powder.
Embodiment 2
Get Fructus Choerospondiatis 500 grams, put into the Chinese medicine multi-function extractor, with 10 times 80% ethanol extraction, extract 4 times, each 3 hours, extracting solution merged, and reclaimed ethanol to the greatest extent, obtained not having pure clear paste, and filter residue and drying is standby; Get no pure clear paste, drying, last HP-10 type macroporous adsorptive resins is with the distilled water eluting of 12 times of column volumes, eluent is standby, and reuse concentration 80%, 8 times of column volume ethanol elutions are collected eluent, reclaim ethanol to the greatest extent, obtain Fructus Choerospondiatis total flavones 34.49 grams, standby; Get dry filtering residue and water elution liquid and merge, put into the Chinese medicine multi-function extractor, add 8 times of water, extract 4 times, each 4 hours, merge extractive liquid,, being evaporated to relative density is 1.20 (50 ℃), adds ethanol and makes determining alcohol reach 70% (V/V), staticly settles, filter, filtrate adds ethanol again makes determining alcohol reach 90% (V/V), staticly settles, filter, merge precipitation, the precipitation dissolved in distilled water, make in the solution every milliliter to amount to raw medicinal herbs 1 gram, after the filtration, with the ultrafilter membrane ultrafiltration of molecular cut off 3,000 5 times, during each ultrafiltration to 1/3, adding distil water is to original volume, concentrated solution, concentrated solution reuse molecular cut off is 100,000 ultrafilter membrane ultrafiltration 5 times, during each ultrafiltration to 1/3, adding distil water is to original volume, collect ultrafiltrate, vacuum concentration, making the solution pol is 5%, obtain Fructus Choerospondiatis water soluble polysaccharide concentrated solution 86.21 grams, standby.Get Fructus Choerospondiatis total flavones and freeze-dried excipient sucrose 404.08 grams and be dissolved in the Fructus Choerospondiatis water soluble polysaccharide concentrated solution, filter, in the packing cillin bottle, be prepared into the Fructus Choerospondiatis freeze-dried powder by the requirement lyophilization of Chinese medicine lyophilized injectable powder with the 0.45um microporous filter membrane.
Embodiment 3
Get Fructus Choerospondiatis 800 grams, put into the Chinese medicine multi-function extractor, with 7 times 60% ethanol extraction, extract 3 times, each 3 hours, extracting solution merged, and reclaimed ethanol to the greatest extent, obtained not having pure clear paste, and filter residue and drying is standby; Get no pure clear paste, drying, last HP-20 type macroporous adsorptive resins, with the distilled water eluting of 9 times of column volumes, eluent is standby, and reuse concentration 40%, 7 times of column volume ethanol elutions are collected eluent, reclaim ethanol to the greatest extent, obtain Fructus Choerospondiatis total flavones 55.18 grams, and are standby; Get dry filtering residue and water elution liquid and merge, put into the Chinese medicine multi-function extractor, add 7 times of water, extract 3 times, each 3 hours, merge extractive liquid,, being evaporated to relative density is 1.16 (50 ℃), adds ethanol and makes alcoholic degree reach 55% (V/V), staticly settles, filter, filtrate adds ethanol again makes determining alcohol reach 80%, staticly settles, filter, merge precipitation, the precipitation dissolved in distilled water, make in the solution every milliliter to amount to raw medicinal herbs 1 gram, after the filtration, with the ultrafilter membrane ultrafiltration of molecular cut off 3,000 4 times, during each ultrafiltration to 1/2, adding distil water is to original volume, concentrated solution, concentrated solution reuse molecular cut off is 100,000 ultrafilter membrane ultrafiltration 4 times, during each ultrafiltration to 1/2, adding distil water is to original volume, collect ultrafiltrate, vacuum concentration, making the solution pol is 3%, obtain Fructus Choerospondiatis water soluble polysaccharide concentrated solution 137.94 grams, standby.Get Fructus Choerospondiatis total flavones and freeze-dried excipient lactose 1013.88 grams and be dissolved in the Fructus Choerospondiatis water soluble polysaccharide concentrated solution, filter, in the packing cillin bottle, be prepared into the Fructus Choerospondiatis freeze-dried powder by the requirement lyophilization of Chinese medicine lyophilized injectable powder with the 0.45um microporous filter membrane.
Embodiment 4
Get Fructus Choerospondiatis 100 grams, put into the Chinese medicine multi-function extractor, with 8 times 70% ethanol extraction, extract 2 times, each 1 hour, extracting solution merged, and reclaimed ethanol to the greatest extent, obtained not having pure clear paste, and standby, filter residue and drying is standby; Get no pure clear paste, drying, last HP-20 type macroporous adsorptive resins, with the distilled water eluting of 10 times of column volumes, eluent is standby, and reuse concentration 50%, 8 times of column volume ethanol elutions are collected eluent, reclaim ethanol to the greatest extent, obtain Fructus Choerospondiatis total flavones 6.90 grams, and are standby; Get dry filtering residue and water elution liquid and merge, put into the Chinese medicine multi-function extractor, add 8 times of water, extract 4 times, each 2 hours, merge extractive liquid,, being evaporated to relative density is 1.17 (50 ℃), adds ethanol and makes alcoholic degree reach 60% (V/V), staticly settles, filter, filtrate adds ethanol again makes determining alcohol reach 85%, staticly settles, filter, merge precipitation, the precipitation dissolved in distilled water, make in the solution every milliliter to amount to raw medicinal herbs 1 gram, after the filtration, with the ultrafilter membrane ultrafiltration of molecular cut off 3,000 3 times, during each ultrafiltration to 1/2, adding distil water is to original volume, concentrated solution, concentrated solution reuse molecular cut off is 100,000 ultrafilter membrane ultrafiltration 5 times, during each ultrafiltration to 1/3, adding distil water is to original volume, collect ultrafiltrate, vacuum concentration, making the solution pol is 4%, obtain Fructus Choerospondiatis water soluble polysaccharide concentrated solution 17.24 grams, standby.Get Fructus Choerospondiatis total flavones and freeze-dried excipient sucrose 109.97 grams and be dissolved in the Fructus Choerospondiatis water soluble polysaccharide concentrated solution, filter, in the packing cillin bottle, be prepared into the Fructus Choerospondiatis freeze-dried powder by the requirement lyophilization of Chinese medicine lyophilized injectable powder with the 0.45um microporous filter membrane.
Embodiment 5
Get Fructus Choerospondiatis 300 grams, put into the Chinese medicine multi-function extractor, with 9 times 75% ethanol extraction, extract 4 times, each 1 hour, extracting solution merged, and reclaimed ethanol to the greatest extent, obtained not having pure clear paste, and standby, filter residue and drying is standby; Get no pure clear paste, drying, last HP-10 type macroporous adsorptive resins is with the distilled water eluting of 11 times of column volumes, eluent is standby, and reuse concentration 75%, 8 times of column volume ethanol elutions are collected eluent, reclaim ethanol to the greatest extent, obtain Fructus Choerospondiatis total flavones 20.70 grams, standby; Get dry filtering residue and water elution liquid and merge, put into the Chinese medicine multi-function extractor, add 7 times of water, extract 4 times, each 2 hours, merge extractive liquid,, being evaporated to relative density is 1.18 (50 ℃), adds ethanol and makes alcoholic degree reach 65% (V/V), staticly settles, filter, filtrate adds ethanol again makes determining alcohol reach 85% (V/V), staticly settles, filter, merge precipitation, the precipitation dissolved in distilled water, make in the solution every milliliter to amount to raw medicinal herbs 1 gram, after the filtration, with the ultrafilter membrane ultrafiltration of molecular cut off 3,000 5 times, during each ultrafiltration 1/2, adding distil water is to original volume, concentrated solution, concentrated solution reuse molecular cut off is 100,000 ultrafilter membrane ultrafiltration 5 times, during each ultrafiltration 1/2, adding distil water is to original volume, collect ultrafiltrate, vacuum concentration, making the solution pol is 2%, obtain Fructus Choerospondiatis water soluble polysaccharide concentrated solution 51.72 grams, standby.Get Fructus Choerospondiatis total flavones and freeze-dried excipient lactose 256.76 grams and be dissolved in the Fructus Choerospondiatis water soluble polysaccharide concentrated solution, filter, in the packing cillin bottle, be prepared into the Fructus Choerospondiatis freeze-dried powder by the requirement lyophilization of Chinese medicine lyophilized injectable powder with the 0.45um microporous filter membrane.
Embodiment 6
Get Fructus Choerospondiatis 1500 grams, put into the Chinese medicine multi-function extractor, with 10 times 75% ethanol extraction, extract 4 times, each 2 hours, extracting solution merged, and reclaimed ethanol to the greatest extent, obtained not having pure clear paste, and standby, filter residue and drying is standby; Get no pure clear paste, drying, last HP-10 type macroporous adsorptive resins is with the distilled water eluting of 12 times of column volumes, eluent is standby, and reuse concentration 55%, 7 times of column volume ethanol elutions are collected eluent, reclaim ethanol to the greatest extent, obtain Fructus Choerospondiatis total flavones 103.46 grams, standby; Get dry filtering residue and water elution liquid and merge, put into the Chinese medicine multi-function extractor, add 8 times of water, extract 2 times, each 4 hours, merge extractive liquid,, being evaporated to relative density is 1.19 (50 ℃), adds ethanol and makes alcoholic degree reach 50% (V/V), staticly settles, filter, filtrate adds ethanol again makes determining alcohol reach 90%, staticly settles, filter, merge precipitation, the precipitation dissolved in distilled water, make in the solution every milliliter to amount to raw medicinal herbs 1 gram, after the filtration, with the ultrafilter membrane ultrafiltration of molecular cut off 3,000 5 times, during each ultrafiltration 1/2, adding distil water is to original volume, concentrated solution, concentrated solution reuse molecular cut off is 100,000 ultrafilter membrane ultrafiltration 5 times, during each ultrafiltration 1/2, adding distil water is to original volume, collect ultrafiltrate, vacuum concentration, making the solution pol is 2%, obtain Fructus Choerospondiatis water soluble polysaccharide concentrated solution 258.62 grams, standby.Get Fructus Choerospondiatis total flavones and freeze-dried excipient lactose 1212.16 grams and be dissolved in the Fructus Choerospondiatis water soluble polysaccharide concentrated solution, filter, in the packing cillin bottle, be prepared into the Fructus Choerospondiatis freeze-dried powder by the requirement lyophilization of Chinese medicine lyophilized injectable powder with the 0.45um microporous filter membrane.
Embodiment 7
Get Fructus Choerospondiatis 1200 grams, put into the Chinese medicine multi-function extractor, with 10 times 80% ethanol extraction, extract 2 times, each 1 hour, extracting solution merged, and reclaimed ethanol to the greatest extent, obtained not having pure clear paste, and standby, filter residue and drying is standby; Get no pure clear paste, drying, last HP-10 type macroporous adsorptive resins is with the distilled water eluting of 12 times of column volumes, eluent is standby, and reuse concentration 65%, 6 times of column volume ethanol elutions are collected eluent, reclaim ethanol to the greatest extent, obtain Fructus Choerospondiatis total flavones 82.76 grams, standby; Get dry filtering residue and water elution liquid and merge, put into the Chinese medicine multi-function extractor, add 7 times of water, extract 3 times, each 3 hours, merge extractive liquid,, being evaporated to relative density is 1.16 (50 ℃), adds ethanol and makes alcoholic degree reach 70% (V/V), staticly settles, filter, filtrate adds ethanol again makes determining alcohol reach 75%, staticly settles, filter, merge precipitation, the precipitation dissolved in distilled water, make in the solution every milliliter to amount to raw medicinal herbs 1 gram, after the filtration, with the ultrafilter membrane ultrafiltration of molecular cut off 3,000 4 times, during each ultrafiltration 1/2, adding distil water is to original volume, concentrated solution, concentrated solution reuse molecular cut off is 100,000 ultrafilter membrane ultrafiltration 4 times, during each ultrafiltration 1/3, adding distil water is to original volume, collect ultrafiltrate, vacuum concentration, making the solution pol is 3.5%, obtain Fructus Choerospondiatis water soluble polysaccharide concentrated solution 206.89 grams, standby.Getting Fructus Choerospondiatis total flavones and freeze-dried excipient mannitol 1779.29 grams is dissolved in the Fructus Choerospondiatis water soluble polysaccharide concentrated solution, filter with the 0.45um microporous filter membrane, in the packing cillin bottle, be prepared into the Fructus Choerospondiatis freeze-dried powder by the requirement lyophilization of Chinese medicine lyophilized injectable powder.
Claims (7)
1. Fructus Choerospondiatis lyophilized injectable powder, it is characterized in that: this Chinese medicine preparation extracts the Fructus Choerospondiatis total flavones of purification and Fructus Choerospondiatis water soluble polysaccharide and excipient substance by the single medicinal material Fructus Choerospondiatis and forms, wherein the Fructus Choerospondiatis total flavones is the 4-6.5 weight portion, the Fructus Choerospondiatis water soluble polysaccharide is the 10-16.5 weight portion, lyophilized powder excipient 77-86 weight portion, wherein the lyophilized powder excipient is a kind of in sucrose, mannitol or the lactose.
2. Fructus Choerospondiatis lyophilized injectable powder according to claim 1 is characterized in that: Fructus Choerospondiatis total flavones 5 weight portions, Fructus Choerospondiatis water soluble polysaccharide are 15 weight portions, lyophilized powder excipient 80 weight portions,
3, Fructus Choerospondiatis lyophilized injectable powder according to claim 1 and 2 is characterized in that: the lyophilized powder excipient is a mannitol.
4. the preparation method of a Fructus Choerospondiatis lyophilized injectable powder, its feature may further comprise the steps:
(1) get Fructus Choerospondiatis, with 6-10 50%-80% ethanol extraction doubly, extract 2-4 time, each 1-3 hour, extracting solution merged, and reclaimed ethanol to the greatest extent, obtained not having pure clear paste, and filter residue and drying is standby;
(2) getting (1) does not have pure clear paste, drying, and last macroporous adsorptive resins, with the distilled water eluting of 8-12 times of column volume, eluent is standby, and reuse concentration 20%-80%, 6-8 times column volume ethanol elution is collected eluent, reclaims ethanol to the greatest extent, obtains the Fructus Choerospondiatis total flavones;
(3) get dry filtering residue and (2) middle water elution liquid merging in (1), extract each 2-4 hour 2-4 time, merge extractive liquid,, being evaporated to relative density is 1.15-1.20 (50 ℃), adds ethanol and makes the determining alcohol degree reach 50%-70%, staticly settle, filter, filtrate adds ethanol again makes determining alcohol reach 75%-90%, staticly settle, filter, merge precipitation, use dissolved in distilled water, make in the solution every milliliter to amount to raw medicinal herbs 1 gram, after the filtration, filtrate;
(4) get filtrate in (3), the ultrafilter membrane ultrafiltration of usefulness molecular cut off 3000 3-5 time gets concentrated solution; Concentrated solution reuse molecular cut off is 100,000 ultrafilter membrane ultrafiltration 3-5 time, collects filtrate, and vacuum concentration obtains Fructus Choerospondiatis water soluble polysaccharide concentrated solution;
(5) get Fructus Choerospondiatis total flavones and freeze-dried excipient and be dissolved in Fructus Choerospondiatis water soluble polysaccharide concentrated solution, filter, in the packing cillin bottle, be prepared into the Fructus Choerospondiatis freeze-dried powder by the requirement lyophilization of Chinese medicine lyophilized injectable powder with the 0.45um microporous filter membrane.
5. according to claim 4, described macroporous adsorbent resin is a HP type macroporous adsorbent resin.
6. according to claim 4,5 described preparation methoies, it is characterized in that: macroporous adsorbent resin is separated into HP-10 type macroporous adsorbent resin to be separated.
7. according to claim 4, when described hyperfiltration process was the 1/2-1/3 of original liquid volume for ultrafiltration and concentration liquid is long-pending, adding distil water continued ultrafiltration to original volume.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101983585A (en) * | 2010-10-28 | 2011-03-09 | 陕西科技大学 | Buccal tablet of jujube alcohol extract and preparation method thereof |
| CN101288468B (en) * | 2008-05-23 | 2011-07-20 | 山西省农业科学院农产品综合利用研究所 | Method of sequential extraction of biological activity component from jujube |
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2004
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101288468B (en) * | 2008-05-23 | 2011-07-20 | 山西省农业科学院农产品综合利用研究所 | Method of sequential extraction of biological activity component from jujube |
| CN101983585A (en) * | 2010-10-28 | 2011-03-09 | 陕西科技大学 | Buccal tablet of jujube alcohol extract and preparation method thereof |
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| Publication number | Publication date |
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| CN1241588C (en) | 2006-02-15 |
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