CN101757129B - Composition preparation containing orientin and isoorientin and preparation method thereof - Google Patents
Composition preparation containing orientin and isoorientin and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a composition preparation containing orientin and isoorientin and a preparation method thereof. The composition preparation is produced by purifying after separately extracting 1-10 parts of polygonum orientale and 1-10 parts of erigeron breviscapus. In the preparation method, a crude extract obtained from polygonum orientale by combination of alcohol extraction and water extraction is purified to be an extract of orientin and isoorientin by extraction with n-butanol and impurity removal with polyamide; and a crude extract obtained from erigeron breviscapus by ethanol extraction is purified to be a total flavonoid extract from erigeron breviscapus by adjusting deposition with acids and alkalies. Compared with the prior art, while effectively reducing adverse drug reactions and enhancing efficacy of the drug, the preparation method of the invention simplifies the production process, reduces the cost and is easy to operate, so as to obtain products with effective and safe clinical application, good stability and high bioavailability, thereby enhancing and ensuring the quality of the products.
Description
Technical field
The present invention relates to a kind of composite preparation that contains orientin and isorientin and preparation method thereof, belong to the technical field of herbal pharmaceutical.
Technical background
Angina pectoris is meant because coronary atherosclerosis or spasm cause myocardial ischemia, the caused angina pectoris of anoxia, accounts for 90% of patient with angina pectoris.It belongs to one of human major disease, and its mortality rate is first of the major disease always.Angina pectoris was mainly in middle-older patient in the past, along with the development of society, and growth in the living standard, its age of onset is tending towards rejuvenation.Therefore, the gesture of evidence of coronary heart diseases trend raising, the task of preventing and treating is very heavy, has caused domestic and international concern.Along with development of modern science and technology, people have also obtained some progress to coronary heart disease diagnosis and control, drug treatment, on the basis of coronary artery dilating (nitrate, nitrous acid ester), the application of calcium ion antagonist, beta-blocker, thrombolytic drug has appearred, for the treatment angina pectoris provides multiple means.Yet clinical practice shows that the simple western medicine treatment is only cured the symptoms, not the disease, and especially side effects of pharmaceutical drugs make the patient be difficult to accept and take for a long time.The hope that the contemporary mankind goes back to nature is strong day by day, generally wishes to accept the treatment by Chinese herbs of natural nuisance-free, thereby provides excellent opportunity for the development of Chinese medicine.Angina pectoris is referred to as obstruction of qi in the chest and cardialgia in the traditional Chinese medical science, the pure Chinese medicinal preparation of developing a kind of efficient, low toxicity, steady quality, dosage form advanced person's treatment angina pectoris is a purpose of the present invention.The angina pectoris state of an illness breaks with tremendous force, and patient's body and mind is caused great injury, therefore, usually needs a kind of relief of symptoms rapidly, releasing patient misery, rapid, the outstanding effect medicine of onset clinically.
Chinese patent 02128066.5 has been reported a kind of Chinese medicine preparation that Herba Polygoni Orientalis 1-50, Herba Erigerontis 50-0 are made, following technology is adopted in the preparation of said preparation: Herba Polygoni Orientalis, Herba Erigerontis decocting in water, precipitate with ethanol are handled, use ethyl acetate extraction then, n-butanol extraction, the isolating method of polyamide column obtains extract.With Herba Polygoni Orientalis and Herba Erigerontis co-extracted, Herba Erigerontis also adopts ethyl acetate extraction and n-butanol extraction therein in this technology, so caused the loss of effective ingredient.
In the patent No. 200610051009.0, optimization and improvement at the deficiencies in the prior art and technology, the inventor carries out water boiling and extraction respectively with Herba Polygoni Orientalis and Herba Erigerontis, Herba Polygoni Orientalis is extracted the back and carries out separation and purification with ethyl acetate, n-butyl alcohol and polyamide column, and the Herba Erigerontis decocting utilizes flavone compound to separate out precipitation under acid condition after boiling, water insoluble, dissolved character purification refine under neutral and weak basic condition.This technology has kept active ingredient preferably, and simplified operating procedure, but the inventor is in process optimization and the improved process, also find to adopt alcohol, water in conjunction with extraction Herba Polygoni Orientalis, Herba Erigerontis adopts alcohol extraction, adopts different steps to carry out purification refine then, the extract effective ingredient that obtains is higher, impurity content is lower, and drug action is good, more helps the preparation of ejection preparation.
Summary of the invention
The objective of the invention is to: a kind of composite preparation that contains orientin and isorientin and preparation method thereof is provided, and said preparation is based on ejection preparation; The present invention investigates we's clinical practice, prescription and herb resource, utilize modern technologies that the quality of preparation Chinese crude drug, preparation process, active constituent content etc. are studied, has the technology advanced person, clinical practice is safe and effective, quality controllable, the bioavailability height, determined curative effect, advantages such as good stability.
The present invention constitutes like this: according to listed as parts by weight, the above-mentioned composite preparation that contains orientin and isorientin is to be prepared from acceptable dosage form on aqueous injection, infusion solution, injectable powder, lyophilized preparation and other pharmaceutics by 1～10 part of 1～10 part of raw material of Chinese medicine Herba Polygoni Orientalis and Herba Erigerontis through extraction.
Preferred proportioning is: Herba Polygoni Orientalis 3-8 part Herba Erigerontis 1-5 part
Most preferred proportioning is: 1 part of 5 parts of Herba Erigerontis of Herba Polygoni Orientalis
Chinese medicine preparation of the present invention, it is the step preparation that Herba Polygoni Orientalis and Herba Erigerontis extract respectively, described step comprises that further the extract that obtains after will be respectively extracting merges, and is active constituents of medicine with the extract of this merging, is prepared into preparation according to the galenic pharmacy routine techniques.
Described extraction respectively, step is as follows: step 1) Herba Polygoni Orientalis alcohol reflux, filter, it is standby that recovery ethanol gets alcohol extract; Medicinal residues decoct with water, and filter, and filtrate concentrates, precipitate with ethanol filters, and reclaims ethanol, filtrate and alcohol extract merge, and transfer pH value, use n-butanol extraction, merge n-butyl alcohol liquid, wash with water, reclaim n-butyl alcohol, residue adds dissolve with ethanol, and last polyamide column is collected stream and worn liquid and eluent, reclaim ethanol, the residue vacuum drying gets orientin and isorientin extract;
Step 2) Herba Erigerontis alcohol reflux filters, and filtrate recycling ethanol also concentrates, and adds water, leaves standstill, and transfers PH, abandons supernatant, and precipitation washes with water, and drying gets the Herba Erigerontis total flavones extract.
Above step further comprises orientin, isorientin extract and Herba Erigerontis total flavones extract is merged, according to the galenic pharmacy routine techniques, makes the step of described Chinese medicine preparation.
Composite preparation of the present invention, preparation method is: step 1) Herba Polygoni Orientalis alcohol reflux, filter, filtrate recycling ethanol also concentrates, and it is standby to get alcohol extract; Medicinal residues decoct with water, and filter, and concentrate precipitate with ethanol, leave standstill, filter, filtrate recycling ethanol also concentrates, filtrate and alcohol extract merge, and transfer PH with hydrochloric acid, use water saturated n-butanol extraction then, merge n-butyl alcohol liquid, wash with water, reclaim n-butyl alcohol, residue adds dissolve with ethanol, and last polyamide column is collected stream and worn liquid and eluent, reclaim ethanol, the residue vacuum drying gets orientin and isorientin extract;
Step 2) Herba Erigerontis alcohol reflux filters, and filtrate recycling ethanol also concentrates, and adds water, leaves standstill, and transfers PH with hydrochloric acid, insulation, and the tipping supernatant, sucking filtration, precipitation washes with water, and drying gets the Herba Erigerontis total flavones extract;
Step 3) said extracted thing adds the injection water, and stirring makes molten, adds glycerol again, and mixing is transferred PH6.8-7.8 with saturated sodium carbonate, adds water for injection, and mixing filters with microporous filter membrane, the filtrate sterile filling, and sterilization promptly gets injection.
Preferred step 1) is: Herba Polygoni Orientalis adds 8-12 times of 50-80% soak with ethanol 10-14 hour, reflux, extract, 1-3 time, each 0.5-2 hour, merge extractive liquid,, filter, filtrate recycling ethanol and when being concentrated into to 50 ℃ relative density be 1.04-1.06, alcohol extract is standby; Medicinal residues add 8-12 times of decocting and boil 2-4 time, and each 1-2 hour, merge extractive liquid,, filter, relative density was 1.05-1.07 when filtrate decompression was concentrated into 50 ℃, added ethanol and made and contain the alcohol amount and reach 50-75%, stir, left standstill 10-24 hour, sucking filtration, decompression filtrate recycling ethanol and when being concentrated into 50 ℃ relative density be 1.04-1.06, merge with aforementioned alcohol extract, transfer PH1-4.5 with hydrochloric acid,, merge n-butyl alcohol liquid with the saturated n-butanol extraction of 1/4-1 times of water gaging 2-6 time, wash 1-3 time with 1/16-1/2 times of water gaging, reclaim under reduced pressure n-butyl alcohol, residue add 60-90% ethanol 2500ml dissolving, last polyamide column, column parameter is 10-1000g, Φ 4-10cm, blade diameter length ratio 1: 2-10, absorption flow velocity: 0.5-4.0BV/h, collect stream and wear liquid and eluent, reclaim ethanol, the residue vacuum drying gets orientin and isorientin extract;
Preferred step 2) be: Herba Erigerontis adds 6-10 times of 50-70% soak with ethanol 10-14 hour, reflux, extract, 2-4 time, each 0.5-2 hour, filter, merging filtrate, filtrate recycling ethanol and when being evaporated to 50 ℃ relative density be 1.10-1.12, add water, constantly stir, left standstill 10～24 hours, sucking filtration, filtrate is transferred PH1～4.5,55 ℃ insulation 2～10 hours with hydrochloric acid, the tipping supernatant, sucking filtration, precipitation washes with water to PH2～5, vacuum drying gets the Herba Erigerontis total flavones extract;
Further comprise step 3), step 3) is: orientin, isorientin extract and Herba Erigerontis total flavones extract are merged, add the injection water, stirring makes molten, add glycerol again, mixing is transferred PH6.8-7.8 with saturated sodium carbonate, add water for injection, mixing filters the filtrate sterile filling with microporous filter membrane, sterilization promptly gets injection.
Preferred step 1) is: Herba Polygoni Orientalis adds 10 times of amount 70% soak with ethanol 12 hours, reflux, extract, 2 times, each 1 hour, merge extractive liquid, filtered, filtrate recycling ethanol and when being concentrated into to 50 ℃ relative density be 1.04-1.06, alcohol extract is standby; Medicinal residues add 10 times of decoctings and boil 3 times, and each 1 hour, merge extractive liquid,, filter, relative density was 1.05-1.07 when filtrate decompression was concentrated into 50 ℃, added ethanol and made and contain the alcohol amount and reach 65%, stir, left standstill 12 hours, sucking filtration, decompression filtrate recycling ethanol and when being concentrated into 50 ℃ relative density be 1.04-1.06, merge with aforementioned alcohol extract, transfer PH3 with hydrochloric acid,, merge n-butyl alcohol liquid with the saturated n-butanol extraction of 1/2 times of water gaging 4 times, wash 2 times with 1/8 times of water gaging, reclaim under reduced pressure n-butyl alcohol, residue add 80% ethanol 2500ml dissolving, last polyamide column, column parameter is 500g, Φ 8cm, blade diameter length ratio 1: 6, absorption flow velocity: 1.5BV/h, collect stream and wear liquid and eluent, reclaim ethanol, the residue vacuum drying gets orientin and isorientin extract;
Step 2) be: Herba Erigerontis adds 8 times of 65% soak with ethanol 12 hours, reflux, extract, 3 times, each 1 hour, filter, merging filtrate, filtrate recycling ethanol and when being evaporated to 50 ℃ relative density be 1.10-1.12, add 1000 milliliters in water, constantly stir, left standstill 12 hours, sucking filtration, filtrate is transferred PH2 with hydrochloric acid, and 55 ℃ are incubated 6 hours, the tipping supernatant, sucking filtration, precipitation washes with water to PH3～4, vacuum drying gets the Herba Erigerontis total flavones extract;
Step 3) is with orientin, isorientin extract and the merging of Herba Erigerontis total flavones extract, to add 1800 milliliters of waters for injection, stirring makes molten, and it is an amount of to add glycerol again, mixing, transfer PH6.8-7.8 with saturated sodium carbonate, add water for injection to 10000 milliliter, mixing filters with 0.45um and 0.22um microporous filter membrane, the filtrate sterile filling, every 10ml sterilized 60 minutes down, promptly gets 1000 injection for 105 ℃.
Function of the present invention cures mainly: have blood circulation promoting and blood stasis dispelling, coronary circulation-promoting pain-relieving function.Be used for the angina pectoris heart blood silt, disease is seen uncomfortable in chest, stabbing pain over the chest does not fixingly move, palpitation and uneasiness, and words are dark violet, and angina pectoris such as thready and hesitant pulse are seen above-mentioned patient.Range of application: this medicament is used for the angina pectoris heart blood silt, and disease is seen stabbing pain over the chest, uncomfortable in chest, and fix and do not move, palpitation and uneasiness, words are dark violet, and angina pectoris such as thready and hesitant pulse are seen above-mentioned patient.
Compared with prior art, the present invention is directed to the physicochemical property of medical material, Herba Polygoni Orientalis and Herba Erigerontis have been adopted the method for extracting respectively.Herba Polygoni Orientalis is adopted alcohol, the bonded thick extraction of water, and precipitate with ethanol, n-butyl alcohol, the purified method of polyamide multiple stage separation prepare orientin and isorientin extract; Herba Erigerontis is adopted alcohol extraction, and the method for different PH separation and purification prepares the Herba Erigerontis total flavones extract, has the technology advanced person, and clinical practice is safe and effective, and is quality controllable, bioavailability height, determined curative effect, advantages such as good stability.
In order to make those of ordinary skills better understand the present invention, below reach composition, the Preparation Method And The Use that embodiment further sets forth present composition preparation by experiment:
One, the selection of technology of the present invention
1, Herba Polygoni Orientalis Study on extraction
1.1 extraction choice of Solvent
Take by weighing Herba Polygoni Orientalis medical material 50g respectively, employing decocts with water, medicinal residues decoct with water three kinds of methods and extract behind the alcohol reflux, alcohol reflux, with extracting solution color and luster, filtration complexity, orientin, isorientin extraction ratio and total solid matters yield serves as to investigate index, studies extracting solvent.
Table 1 Herba Polygoni Orientalis extraction process table
Experimental result shows that employing alcohol, moisture are put forward the method that combines and extracted the Herba Polygoni Orientalis medical material, and extracting solution is all obtained good result at aspects such as color and luster, content, filtration difficulty or ease.Though adopt the content of alcohol extraction also higher separately, consider the refining pure metallization processes of next stage, preferred alcohols, water combination.
1.2 alcohol extraction process research
A. extraction time is investigated
Sample preparation: get Herba Polygoni Orientalis medical material 50g, add 70% alcohol heating reflux 4 times, each 1 hour, collect each backflow respectively, filter.With orientin and isorientin total amount extraction ratio is that index is investigated:
Table 2 extraction time-total solid yield table
| Extraction time | 1 | 2 | 3 | 4 |
| Total amount (%) | 78.52 | 82.73 | 83.81 | 84.32 |
Data show in the table, when extracting four times, the total solid yield has not almost had big variation in the Herba Polygoni Orientalis, determines that therefore extraction time is 1-3 time, wherein extracts 2 times and is optimised process, and less expensive is reasonable.
B. extract the investigation of amount of alcohol
Sample preparation: get Herba Polygoni Orientalis 50g, comply with 70% different ethanol of surface condition adding down, reflux 2 times, each 1 hour, filter, collect filtrate.The result is as follows:
Table 3 extracted amount-total solid yield table
| Amount of alcohol is the medical material multiple | 4 | 6 | 8 | 10 | 12 | 14 |
| Total amount (%) | 75.29 | 77.11 | 80.83 | 82.44 | 83.69 | 84.07 |
The total solid yield increases with the increasing of amount of alcohol, but not have bigger increase to back to a certain degree, thus select alcoholic acid amount be medical material 8-12 doubly, preferably addition is 10 times of amounts.
C. the investigation of concentration of alcohol
Sample preparation: get Herba Polygoni Orientalis 50g, comply with surface condition adding Different concentrations of alcohol down, reflux 2 times, each 1 hour, filter, collect filtrate.The result is as follows:
Table 4 concentration of alcohol-total solid yield table
| Concentration of alcohol (%) | 40 | 50 | 60 | 70 | 80 | 90 |
| Total amount (%) | 75.65 | 79.61 | 80.48 | 82.27 | 83.74 | 83.16 |
The total solid yield increases with the increasing of concentration of alcohol, is increased to 90% total recovery decline on the contrary but work as concentration, and therefore selecting concentration of alcohol is 50-80%, is preferably 70%.
In addition, the applicant finds under study for action, soaks 10-14 hour before the Herba Polygoni Orientalis medicinal material extract, and the extraction of its orientin, isorientin etc. is more complete.So comprehensive The above results, the alcohol extraction process of decision Herba Polygoni Orientalis medical material is: with 50%-80% soak with ethanol 10-14 hour, reflux, extract, was 1-3 time then, at every turn 8-12 doubly measure, 0.5-2 hour.Be preferably: with 70% soak with ethanol 12 hours, reflux, extract, 2 times, each 10 times of amounts, 1 hour.
1.3 extraction process by water research
Medicinal residues behind the alcohol reflux being carried out water boiling and extraction, boil technology with reference to the decocting of inventor Herba Polygoni Orientalis in the patent No. 200610051009.0, is index with orientin, isorientin, total solid matters yield, investigates the stability and the reasonability of technology.
A. extraction time is investigated
Medicinal residues are added 10 times of water gagings, and the according to the form below number of times extracts, and each 1 hour is index with total solid, orientin, isorientin extraction ratio, investigates the influence of extraction time to the medical material effective component extraction rate.
Table 5 extraction time-extraction ratio evaluation table
| Amount of water is the medical material multiple | 1 | 2 | 3 | 4 | 5 |
| Orientin extraction ratio (%) | 1.14 | 1.52 | 1.74 | 1.83 | 1.88 |
| Isorientin extraction ratio (%) | 0.81 | 1.23 | 1.40 | 1.52 | 1.55 |
| Total solid extraction ratio (%) | 0.16 | 0.30 | 0.42 | 0.48 | 0.49 |
The result shows that extraction ratio increases with the increase of extraction time, but does not have bigger increase to back to a certain degree, so selective extraction 2-4 time is preferably extracted 3 times, less expensive is reasonable.
B. amount of water is investigated
Medicinal residues behind the ethanol extraction, according to the form below amount of water extract respectively 3 times, and each 1 hour is index with the total solid extraction ratio, investigate the influence of amount of water to the medical material effective component extraction rate.
Table 6 amount of water-total solid extraction ratio evaluation table
| The amount of water multiple | 6 | 8 | 10 | 12 | 14 |
| Total solid extraction ratio (%) | 0.31 | 0.43 | 0.50 | 0.54 | 0.56 |
The result shows that extraction ratio increases with the increasing of amount of water, but does not have bigger increase after to a certain degree, is 8-12 times so select amount of water, and preferred addition is 10 times of amounts, economical rationality.
2, Herba Polygoni Orientalis process for refining research
In the process modification process, the inventor adopts ethyl acetate extraction with the crude extract of Herba Polygoni Orientalis, n-butanol extraction, cross the mode remove impurity of polyamide column at last, its complex operation, simultaneously half-finished relative density, pH value etc. all there is requirement, the inventor is through repeatedly test and to the reference of document, remove the step of ethyl acetate extraction, result of the test shows, the rate of transform of effective ingredient, the color and luster of medicinal liquid, clarity did not influence are simultaneously because work simplification, save production time and production cost, be fit to big requirement of producing.In orientin in the crude extract before refining is 100%, and the result is as follows:
The different purification conditions of table 7 are table as a result
| Technology | Before refining | Ethyl acetate+n-butyl alcohol+polyamide | N-butyl alcohol+polyamide |
| The plain rate of transform of red grass (%) | 100 | 96.57 | 96.32 |
| Color and luster | Brown | Light brown | Light brown |
| Clarity | Clear and bright | Clear and bright | Clear and bright |
3, Herba Erigerontis Study on extraction
3.1 extraction choice of Solvent
Take by weighing Herba Erigerontis medical material 10g respectively, adopt decoct with water, alcohol reflux, the ethyl acetate three kinds of methods that reflux are extracted, and serve as to investigate index with extracting solution color and luster, clarity, scutellarin content, study extracting solvent.
Table 8 Herba Erigerontis extraction process table
| Method | Evaluation index | Scutellarin content (mg/g) | Clarity | Color and luster |
| 1 | Water is carried | 5.25mg/g | Clear and bright | Brown |
| 2 | Alcohol extraction | 5.76mg/g | Clear and bright | Light brown |
| 3 | Ethyl acetate extraction | 4.68mg/g | Slightly muddy | Pale brown color |
Experimental result shows, adopts the sample of ethyl acetate extraction, and pigment is heavier, and it is bigger to measure the loss of active ingredients rate during subsequent technique is handled, and alcohol reflux Herba Erigerontis medical material, extracting solution is all obtained good result at aspects such as color and luster, content, clarity.So select ethanol for extracting solvent.
3.2 alcohol extraction process research
A. extraction time is investigated
Sample preparation: get Herba Erigerontis medical material 10g, add 60% alcohol heating reflux 5 times, each 1 hour, collect each backflow respectively, filter.
Table 9 extraction time-scutellarin yield table
| Extraction time | 1 | 2 | 3 | 4 | 5 |
| Scutellarin (mg/g) | 3.81 | 4.90 | 5.34 | 5.66 | 5.70 |
Data show in the table, when extracting four times, the scutellarin yield has not almost had big variation in the Herba Erigerontis, determines that therefore extraction time is 2-4 time, wherein extracts 3 times and is optimised process, and less expensive is reasonable.
B. extract the investigation of amount of alcohol
Sample preparation: get Herba Erigerontis 10g, comply with 65% not commensurability ethanol of surface condition adding down, reflux 3 times, each 1 hour, filter, collect filtrate.The result is as follows:
Table 10 extracted amount-total solid yield table
| Amount of alcohol is the medical material multiple | 4 | 6 | 8 | 10 | 12 | 14 |
| Scutellarin (mg/g) | 4.48 | 5.23 | 5.46 | 5.60 | 5.64 | 5.68 |
The scutellarin yield increases with the increasing of amount of alcohol, but not have bigger increase to back to a certain degree, thus select alcoholic acid amount be medical material 6-10 doubly, preferably addition is 8 times of amounts.
C. the investigation of concentration of alcohol
Sample preparation: get Herba Erigerontis 10g, comply with the ethanol of 8 times of amounts of surface condition adding variable concentrations down, reflux 3 times, each 1 hour, filter, collect filtrate.The result is as follows:
Table 11 concentration of alcohol-total solid yield table
| Concentration of alcohol (%) | 45 | 50 | 55 | 60 | 65 | 70 | 75 |
| Scutellarin (mg/g) | 4.86 | 5.27 | 5.53 | 5.62 | 5.71 | 5.75 | 5.77 |
The scutellarin yield increases with the increasing of concentration of alcohol, but does not have bigger increase after 70% when concentration is increased to, and therefore selecting concentration of alcohol is 50-70%, is preferably 65%.
In addition, the applicant finds under study for action, soaks 10-14 hour before the Herba Erigerontis medicinal material extract, and the extraction of effective ingredient such as its scutellarin is more complete.So comprehensive The above results, the alcohol extraction process of decision Herba Erigerontis medical material is: with 50%-70% soak with ethanol 10-14 hour, reflux, extract, was 2-4 time then, at every turn 8-10 doubly measure, 0.5-2 hour.Be preferably: with 65% soak with ethanol 12 hours, reflux, extract, 3 times, each 8 times of amounts, 1 hour.
4, Herba Erigerontis extract process for refining research
The inventor is according to the accumulation of technical study and to the investigation of lot of documents, and the alcohol extract of Herba Erigerontis is adopted the dried solution remove impurity of 1% albumen, and ethyl acetate extraction, aqueous solution are regulated modes such as soda acid sedimentation remove impurity, investigate the purification refine technology of extract.Is 100% in alcohol extract before refining, and the result is as follows:
Table 12 different solvents purifying process table
| Technology | Alcohol extract | The dried solution of 1% albumen | Ethyl acetate | Acid-alkali accommodation |
| The scutellarin rate of transform (%) | 100 | 93.6 | 94.8 | 96.3 |
More than test shows, utilizes flavone compound to separate out precipitation under acid condition, and is water insoluble, dissolved character under neutral and weak basic condition, employing is dissolved in water, natural subsidence, the mode purification refine Herba Erigerontis extract of adjusting soda acid remove impurity, be very rational, and organic solvent residue can be brought hidden danger for the preparation of follow-up ejection preparation, so the mode of acid-alkali accommodation is not only simplified production technology, reduces cost, and easy and simple to handle, be to be fit to big refining mode of producing.
Two, Herba Polygoni Orientalis and erigeron breviscapus composition preparation are to the effect of rat experiment myocardial ischemia
2.1 medicine: XIANGDAN ZHUSHEYE, lot number 040706 Pharmacuetical Plant of Huaxi Medical Univ. produces, positive contrast medicine 1; The injection use compound Herba Polygoni Orientalis is according to the patent No. 200610051009.0 described method preparations, positive contrast medicine 2; Compound oriental smartweed injection by preparation method of the present invention is made is medicine of the present invention.
Animal: SD male rat.
2.2 experimental technique and result
Get the SD male rat, be divided into 4 groups at random, according to following table dosage grouping administration.Animal Anesthesia, fixing before the test, the record normal ECG.Connect artificial respirator before opening the thoracic cavity, behind the ligation left coronary artery descending branch, close the thoracic cavity rapidly, recover to breathe, recording ecg has the obvious ST section person of raising to be the successful sign of operation (reject and obvious myocardial infarction electrocardiographic wave person do not occur).Each group is femoral vein administration 6.0g/kg respectively, and the normal saline matched group is given with the volume normal saline.Record ligation larynx 10,30, each time point electrocardiogram of 120min calculate each time ST section and are offset total mv number up and down, and carry out statistical disposition, the results are shown in Table 13.After the off-test, take out heart immediately, wash surplus blood with normal saline, cut atrium and each trunk, fascia, auricle, take by weighing ventricular weight, then cardiac muscle is cut into 5 of equal thickness, place 37 ℃ of 0.5%N-BT dyeing body fluid 10min that dyes, taking-up cuts off the non-infarcted myocardium that is colored, the undyed infarcted myocardium of weighing is by formula: myocardial ischemia percentage ratio=ischemic region weight ÷ ventricular weight * 100%, calculating myocardium ischemic region percentage rate, carry out statistical disposition, the results are shown in Table 14.
The influence of ECG behind the table 13 pair rat ligation ramus descendens anterior arteriae coronariae sinistrae (X ± SD)
Compare with the N.S matched group
*P＜0.05
*P＜0.01
The influence of table 14 pair rat acute myocardial infarct size (X ± SD)
| Sample | Dosage g/kg | Number of animals (only) | Ventricle heavy (g) | Infarction heavy (g) | Infarction weight/ventricle heavy (%) |
| The N.S matched group | - | 9 | 0.83±0.22 | 0.19±0.08 | 21.84±10.15 |
| Positive controls 1 | 6.0 | 9 | 0.66±0.10 | 0.07±0.04 * | 12.16±4.20 ** |
| Positive controls 2 | 6.0 | 9 | 0.67±0.14 | 0.10±0.03 * | 14.80±6.16 ** |
| Medicine of the present invention | 6.0 | 9 | 0.65±0.11 | 0.08±0.02 * | 13.58±5.56 ** |
Compare with the N.S matched group
*P＜0.05
*P＜0.01
Result of the test shows, compound oriental smartweed injection of the present invention and existing ejection preparation and the technology of applying for a patent compare, can obviously improve action effect to the rat experiment myocardial ischemia, and existing relatively therapeutic equivalence, with respect to the research technology before the applicant, the better efficacy of ejection preparation of the present invention, bioavailability is higher.
2.3 experiment is got mice by table 15 grouping and dosed administration to mice normal pressure anoxia enduring, each administration group administration 0.1ml/, matched group is given equivalent N.S, behind the 10min, put into the wide mouthed bottle of putting the 15g sodica calx in advance, the record mouse diing time, carry out statistical procedures, the results are shown in Table 15.
The influence of table 15 pair mice normal pressure hypoxia endurance time (X ± SD)
| Group | Dosage g/kg | Number of animals (only) | Death time (min) |
| The N.S matched group | - | 10 | 40.3±14.09 |
| Positive controls 1 | 10 | 10 | 52.1±10.23 * |
| Positive controls 2 | 10 | 10 | 51.6±11.58 * |
| Medicine of the present invention | 10 | 10 | 54.5±10.44 * |
Compare with the N.S matched group
*P＜0.05
*P＜0.01
Result of the test shows that Herba Polygoni Orientalis of the present invention and erigeron breviscapus composition preparation have obvious resisting oxygen lack, with the normal saline group more all have significant difference (
*P＜0.01), compares therapeutic equivalence, be better than positive control 2 with positive control 1.
More than test shows that Herba Polygoni Orientalis of the present invention and erigeron breviscapus composition preparation can obviously improve the ischemic myocardial electrocardiogram, and the rat acute myocardial infarction is had obvious protective effect, and is comparatively obvious to the resisting oxygen lack under the mice normal pressure simultaneously.The resulting product determined curative effect of technology of the present invention is described, clinical practice is safe and effective, and good stability is quality controllable, the bioavailability height, and technology is rationally advanced.
The specific embodiment:
Need to prove that this preparation embodiment introduces a kind of method for preparing extract, is in order to explain the present invention, rather than restriction the present invention.
Embodiment 1: the preparation of injection
Raw material: Herba Polygoni Orientalis 7500g, Herba Erigerontis 1500g
Preparation method: step 1) is: Herba Polygoni Orientalis adds 10 times of amount 70% soak with ethanol 12 hours, reflux, extract, 2 times, each 1 hour, merge extractive liquid, filtered, filtrate recycling ethanol and when being concentrated into to 50 ℃ relative density be 1.04-1.06, alcohol extract is standby; Medicinal residues add 10 times of decoctings and boil 3 times, and each 1 hour, merge extractive liquid,, filter, relative density was 1.05-1.07 when filtrate decompression was concentrated into 50 ℃, added ethanol and made and contain the alcohol amount and reach 65%, stir, left standstill 12 hours, sucking filtration, decompression filtrate recycling ethanol and when being concentrated into 50 ℃ relative density be 1.04-1.06, merge with aforementioned alcohol extract, transfer PH3 with hydrochloric acid,, merge n-butyl alcohol liquid with the saturated n-butanol extraction of 1/2 times of water gaging 4 times, wash 2 times with 1/8 times of water gaging, reclaim under reduced pressure n-butyl alcohol, residue add 80% ethanol 2500ml dissolving, last polyamide column, column parameter is 500g, Φ 8cm, blade diameter length ratio 1: 6, absorption flow velocity: 1.5BV/h, collect stream and wear liquid and eluent, reclaim ethanol, the residue vacuum drying gets orientin and isorientin extract;
Step 2) be: Herba Erigerontis adds 8 times of 65% soak with ethanol 12 hours, reflux, extract, 3 times, each 1 hour, filter, merging filtrate, filtrate recycling ethanol and when being evaporated to 50 ℃ relative density be 1.10-1.12, add 1000 milliliters in water, constantly stir, left standstill 12 hours, sucking filtration, filtrate is transferred PH2 with hydrochloric acid, and 55 ℃ are incubated 6 hours, the tipping supernatant, sucking filtration, precipitation washes with water to PH3～4, vacuum drying gets the Herba Erigerontis total flavones extract;
Step 3) is with orientin, isorientin extract and the merging of Herba Erigerontis total flavones extract, to add 1800 milliliters of waters for injection, stirring makes molten, and it is an amount of to add glycerol again, mixing, transfer PH6.8-7.8 with saturated sodium carbonate, add water for injection to 10000 milliliter, mixing filters with 0.45um and 0.22um microporous filter membrane, the filtrate sterile filling, every 10ml sterilized 60 minutes down, promptly gets 1000 of compound oriental smartweed injection for 105 ℃.
Embodiment 2: the preparation of transfusion
Raw material: Herba Polygoni Orientalis 1000g, Herba Erigerontis 5000g
Preparation method: step 1) is: Herba Polygoni Orientalis adds 8 times of 50% soak with ethanol 10 hours, reflux, extract, 0.5 hour, extracting solution filters, filtrate recycling ethanol and when being concentrated into to 50 ℃ relative density be 1.04-1.06, alcohol extract is standby; Medicinal residues add 8 times of decoctings and boil 2 times, and each 1 hour, merge extractive liquid,, filter, relative density was 1.05-1.07 when filtrate decompression was concentrated into 50 ℃, added ethanol and made and contain the alcohol amount and reach 50%, stir, left standstill 10 hours, sucking filtration, decompression filtrate recycling ethanol and when being concentrated into 50 ℃ relative density be 1.04-1.06, merge with aforementioned alcohol extract, transfer PH1 with hydrochloric acid,, merge n-butyl alcohol liquid with the saturated n-butanol extraction of 1/4 times of water gaging 2 times, wash with 1/16 times of water gaging, reclaim under reduced pressure n-butyl alcohol, residue add 60% ethanol 2500ml dissolving, last polyamide column, column parameter is 100g, Φ 4cm, blade diameter length ratio 1: 2, absorption flow velocity: 0.5BV/h, collect stream and wear liquid and eluent, reclaim ethanol, the residue vacuum drying gets orientin and isorientin extract;
Step 2) be: Herba Erigerontis adds 10 times of 70% soak with ethanol 14 hours, reflux, extract, 4 times, each 2 hours, filter, merging filtrate, filtrate recycling ethanol and when being evaporated to 50 ℃ relative density be 1.10-1.12, add water, constantly stir, left standstill 24 hours, sucking filtration, filtrate is transferred PH4.5 with hydrochloric acid, and 55 ℃ are incubated 10 hours, the tipping supernatant, sucking filtration, precipitation washes with water to PH5, vacuum drying gets the Herba Erigerontis total flavones extract;
Step 3) is: orientin, isorientin extract and Herba Erigerontis total flavones extract are merged, add the injection water, stirring makes molten, adds glycerol again, and mixing is transferred PH6.8-7.8 with saturated sodium carbonate, adds water for injection, makes infusion preparation with conventional method.
Embodiment 3: the preparation of lyophilized injectable powder
Raw material: Herba Polygoni Orientalis 3000g, Herba Erigerontis 1000g
Preparation method: step 1) is: Herba Polygoni Orientalis adds 12 times of 80% soak with ethanol 14 hours, reflux, extract, 3 times, each 2 hours, merge extractive liquid, filtered, filtrate recycling ethanol and when being concentrated into to 50 ℃ relative density be 1.04-1.06, alcohol extract is standby; Medicinal residues add 12 times of decoctings and boil 4 times, and each 2 hours, merge extractive liquid,, filter, relative density was 1.05-1.07 when filtrate decompression was concentrated into 50 ℃, added ethanol and made and contain the alcohol amount and reach 75%, stir, left standstill 24 hours, sucking filtration, decompression filtrate recycling ethanol and when being concentrated into 50 ℃ relative density be 1.04-1.06, merge with aforementioned alcohol extract, transfer PH4.5 with hydrochloric acid,, merge n-butyl alcohol liquid with the saturated n-butanol extraction of 1 times of water gaging 6 times, wash 3 times with 1/2 times of water gaging, reclaim under reduced pressure n-butyl alcohol, residue add 90% ethanol 2500ml dissolving, last polyamide column, column parameter is 1000g, Φ 10cm, blade diameter length ratio 1: 10, absorption flow velocity: 4.0BV/h, collect stream and wear liquid and eluent, reclaim ethanol, the residue vacuum drying gets orientin and isorientin extract;
Step 2) be: Herba Erigerontis adds 6 times of 50% soak with ethanol 10 hours, reflux, extract, 2 times, each 0.5 hour, filter, merging filtrate, filtrate recycling ethanol and when being evaporated to 50 ℃ relative density be 1.10-1.12, add water, constantly stir, left standstill 10 hours, sucking filtration, filtrate is transferred PH1 with hydrochloric acid, and 55 ℃ are incubated 2 hours, the tipping supernatant, sucking filtration, precipitation washes with water to PH2, vacuum drying gets the Herba Erigerontis total flavones extract;
Step 3) is: orientin, isorientin extract and Herba Erigerontis total flavones extract are mixed, add the injection water, stirring makes molten, is prepared into lyophilized injectable powder with conventional method.
Embodiment 4: the preparation of injectable powder
Raw material: Herba Polygoni Orientalis 1000g, Herba Erigerontis 100g
Preparation method: step 1) is: Herba Polygoni Orientalis adds 9 times of 60% soak with ethanol 12 hours, reflux, extract, 2 times, each 1.5 hours, merge extractive liquid, filtered, filtrate recycling ethanol and when being concentrated into to 50 ℃ relative density be 1.04-1.06, alcohol extract is standby; Medicinal residues add 9 times of decoctings and boil 4 times, and each 1.5 hours, merge extractive liquid,, filter, relative density was 1.05-1.07 when filtrate decompression was concentrated into 50 ℃, added ethanol and made and contain the alcohol amount and reach 70%, stir, left standstill 18 hours, sucking filtration, decompression filtrate recycling ethanol and when being concentrated into 50 ℃ relative density be 1.04-1.06, merge with aforementioned alcohol extract, transfer PH2-4.5 with hydrochloric acid,, merge n-butyl alcohol liquid with the saturated n-butanol extraction of 1/2 times of water gaging 3 times, wash 2 times with 1/4 times of water gaging, reclaim under reduced pressure n-butyl alcohol, residue add 70% ethanol 2500ml dissolving, last polyamide column, column parameter is 400g, Φ 6cm, blade diameter length ratio 1: 40, absorption flow velocity: 2.0BV/h, collect stream and wear liquid and eluent, reclaim ethanol, the residue vacuum drying gets orientin and isorientin extract;
Step 2) be: Herba Erigerontis adds 9 times of 55% soak with ethanol 12 hours, reflux, extract, 3 times, each 1.5 hours, filter, merging filtrate, filtrate recycling ethanol and when being evaporated to 50 ℃ relative density be 1.10-1.12, add water, constantly stir, left standstill 15 hours, sucking filtration, filtrate is transferred PH1～3,55 ℃ insulation 5 hours with hydrochloric acid, the tipping supernatant, sucking filtration, precipitation washes with water to PH2～4, vacuum drying gets the Herba Erigerontis total flavones extract;
Step 3) is: orientin, isorientin extract and Herba Erigerontis total flavones extract are mixed, add the injection water, stirring makes molten, is prepared into injectable powder with conventional method.
Embodiment 5: the preparation of tablet
Raw material: Herba Polygoni Orientalis 100g, Herba Erigerontis 1000g
Preparation method: step 1) is: Herba Polygoni Orientalis adds 11 times of 75% soak with ethanol 10 hours, reflux, extract, 3 times, each 1 hour, merge extractive liquid, filtered, filtrate recycling ethanol and when being concentrated into to 50 ℃ relative density be 1.04-1.06, alcohol extract is standby; Medicinal residues add 11 times of decoctings and boil 3 times, and each 1 hour, merge extractive liquid,, filter, relative density was 1.05-1.07 when filtrate decompression was concentrated into 50 ℃, added ethanol and made and contain the alcohol amount and reach 55%, stir, left standstill 15 hours, sucking filtration, decompression filtrate recycling ethanol and when being concentrated into 50 ℃ relative density be 1.04-1.06, merge with aforementioned alcohol extract, transfer PH1-3 with hydrochloric acid,, merge n-butyl alcohol liquid with the saturated n-butanol extraction of 3/4 times of water gaging 5 times, wash 3 times with 1/8 times of water gaging, reclaim under reduced pressure n-butyl alcohol, residue add 85% ethanol 2500ml dissolving, last polyamide column, column parameter is 600g, Φ 9cm, blade diameter length ratio 1: 8, absorption flow velocity: 3.0BV/h, collect stream and wear liquid and eluent, reclaim ethanol, the residue vacuum drying gets orientin and isorientin extract;
Step 2) be: Herba Erigerontis adds 7 times of 60% soak with ethanol 14 hours, reflux, extract, 2 times, each 1 hour, filter, merging filtrate, filtrate recycling ethanol and when being evaporated to 50 ℃ relative density be 1.10-1.12, add water, constantly stir, left standstill 18 hours, sucking filtration, filtrate is transferred PH2～4.5,55 ℃ insulation 8 hours with hydrochloric acid, the tipping supernatant, sucking filtration, precipitation washes with water to PH3～5, vacuum drying gets the Herba Erigerontis total flavones extract;
Step 3) is: get orientin, isorientin extract and Herba Erigerontis total flavones extract, mix homogeneously adds adjuvant, granulate, and tabletting, promptly.
Embodiment 6: get Herba Polygoni Orientalis 4000g and Herba Erigerontis 1000g, pulverize, take that arbitrary method obtains orientin, isorientin extract and Herba Erigerontis total flavones extract in the foregoing description, add conventional adjuvant again and be prepared into drop pill.
Embodiment 7: orientin, isorientin extract and Herba Erigerontis total flavones extract with arbitrary method in the foregoing description obtains are prepared into pill with the galenic pharmacy routine techniques.
Embodiment 8: orientin, isorientin extract and Herba Erigerontis total flavones extract that embodiment 1 is obtained mix, and are prepared into capsule with the galenic pharmacy routine techniques.
Embodiment 9: orientin, isorientin extract and Herba Erigerontis total flavones extract that embodiment 4 is obtained mix, and add ethanol system soft material, granulate, and drying, packing gets granule.
Claims (8)
1. composite preparation that contains orientin and isorientin is characterized in that: calculate according to components by weight percent: it is to be prepared from through following preparation method by 1～10 part of 1～10 part of raw material of Chinese medicine Herba Polygoni Orientalis and Herba Erigerontis:
Step 1) Herba Polygoni Orientalis alcohol reflux filters, and it is standby that recovery ethanol gets alcohol extract; Medicinal residues decoct with water, and filter, and filtrate concentrates, precipitate with ethanol filters, and reclaims ethanol, filtrate and alcohol extract merge, and transfer pH value, use n-butanol extraction, merge n-butyl alcohol liquid, wash with water, reclaim n-butyl alcohol, residue adds dissolve with ethanol, and last polyamide column is collected stream and worn liquid and eluent, reclaim ethanol, the residue vacuum drying gets orientin and isorientin extract;
Step 2) Herba Erigerontis alcohol reflux filters, and filtrate recycling ethanol also concentrates, and adds water, leaves standstill, and transfers PH, abandons supernatant, and precipitation washes with water, and drying gets the Herba Erigerontis total flavones extract;
Step 3) merges orientin, isorientin extract and Herba Erigerontis total flavones extract, according to the galenic pharmacy routine techniques, makes described Chinese medicine preparation.
2. contain the composite preparation of orientin and isorientin according to claim 1, it is characterized in that: the weight proportion of crude drug is:
Herba Polygoni Orientalis 3-8 part Herba Erigerontis 1-5 part.
3. contain the composite preparation of orientin and isorientin according to claim 1, it is characterized in that: the weight proportion of crude drug is:
1 part of 5 parts of Herba Erigerontis of Herba Polygoni Orientalis.
4. contain the composite preparation of orientin and isorientin as claim 1-3 as described in arbitrary, it is characterized in that:
Wherein said step 1) is: the Herba Polygoni Orientalis alcohol reflux, filter, and filtrate recycling ethanol also concentrates, and it is standby to get alcohol extract; Medicinal residues decoct with water, and filter, and concentrate precipitate with ethanol, leave standstill, filter, filtrate recycling ethanol also concentrates, filtrate and alcohol extract merge, and transfer PH with hydrochloric acid, use water saturated n-butanol extraction then, merge n-butyl alcohol liquid, wash with water, reclaim n-butyl alcohol, residue adds dissolve with ethanol, and last polyamide column is collected stream and worn liquid and eluent, reclaim ethanol, the residue vacuum drying gets orientin and isorientin extract;
Described step 2) be: the Herba Erigerontis alcohol reflux, filter, filtrate recycling ethanol also concentrates, and adds water, leaves standstill, and transfers PH with hydrochloric acid, insulation, the tipping supernatant, sucking filtration, precipitation washes with water, and drying gets the Herba Erigerontis total flavones extract.
5. as containing the composite preparation of orientin and isorientin as described in the claim 4, it is characterized in that:
Wherein said step 1) is: Herba Polygoni Orientalis adds 8-12 times of 50-80% soak with ethanol 10-14 hour, reflux, extract, 1-3 time, each 0.5-2 hour, merge extractive liquid,, filter, filtrate recycling ethanol and when being concentrated into 50 ℃ relative density be 1.04-1.06, alcohol extract is standby; Medicinal residues add 8-12 times of decocting and boil 2-4 time, and each 1-2 hour, merge extractive liquid,, filter, relative density was 1.05-1.07 when filtrate decompression was concentrated into 50 ℃, added ethanol and made and contain the alcohol amount and reach 50-75%, stir, left standstill 10-24 hour, sucking filtration, decompression filtrate recycling ethanol and when being concentrated into 50 ℃ relative density be 1.04-1.06, merge with aforementioned alcohol extract, transfer PH1-4.5 with hydrochloric acid,, merge n-butyl alcohol liquid with the saturated n-butanol extraction of 1/4-1 times of water gaging 2-6 time, wash 1-3 time with 1/16-1/2 times of water gaging, reclaim under reduced pressure n-butyl alcohol, residue add 60-90% ethanol 2500ml dissolving, last polyamide column, column parameter is 10-1000g, Φ 4-10cm, blade diameter length ratio 1: 2-10, absorption flow velocity: 0.5-4.0BV/h, collect stream and wear liquid and eluent, reclaim ethanol, the residue vacuum drying gets orientin and isorientin extract;
Described step 2) be: Herba Erigerontis adds 6-10 times of 50-70% soak with ethanol 10-14 hour, reflux, extract, 2-4 time, each 0.5-2 hour, filter, merging filtrate, filtrate recycling ethanol and when being evaporated to 50 ℃ relative density be 1.10-1.12, add water, constantly stir, left standstill 10～24 hours, sucking filtration, filtrate is transferred PH1～4.5,55 ℃ insulation 2～10 hours with hydrochloric acid, the tipping supernatant, sucking filtration, precipitation washes with water to PH2～5, vacuum drying gets the Herba Erigerontis total flavones extract.
6. as containing the composite preparation of orientin and isorientin as described in the claim 5, it is characterized in that: comprise that further step 3) is: orientin, isorientin extract and Herba Erigerontis total flavones extract are merged, add the injection water, stirring makes molten, add glycerol again, mixing is transferred PH6.8-7.8 with saturated sodium carbonate, add water for injection, mixing filters the filtrate sterile filling with microporous filter membrane, sterilization promptly gets injection.
7. as containing the composite preparation of orientin and isorientin as described in according to claim 5, it is characterized in that:
Step 1) is: Herba Polygoni Orientalis adds 10 times of amount 70% soak with ethanol 12 hours, reflux, extract, 2 times, each 1 hour, merge extractive liquid, filtered, filtrate recycling ethanol and when being concentrated into 50 ℃ relative density be 1.04-1.06, alcohol extract is standby; Medicinal residues add 10 times of decoctings and boil 3 times, and each 1 hour, merge extractive liquid,, filter, relative density was 1.05-1.07 when filtrate decompression was concentrated into 50 ℃, added ethanol and made and contain the alcohol amount and reach 65%, stir, left standstill 12 hours, sucking filtration, decompression filtrate recycling ethanol and when being concentrated into 50 ℃ relative density be 1.04-1.06, merge with aforementioned alcohol extract, transfer PH3 with hydrochloric acid,, merge n-butyl alcohol liquid with the saturated n-butanol extraction of 1/2 times of water gaging 4 times, wash 2 times with 1/8 times of water gaging, reclaim under reduced pressure n-butyl alcohol, residue add 80% ethanol 2500ml dissolving, last polyamide column, column parameter is 500g, Φ 8cm, blade diameter length ratio 1: 6, absorption flow velocity: 1.5BV/h, collect stream and wear liquid and eluent, reclaim ethanol, the residue vacuum drying gets orientin and isorientin extract;
Step 2) be: Herba Erigerontis adds 8 times of 65% soak with ethanol 12 hours, reflux, extract, 3 times, each 1 hour, filter, merging filtrate, filtrate recycling ethanol and when being evaporated to 50 ℃ relative density be 1.10-1.12, add 1000 milliliters in water, constantly stir, left standstill 12 hours, sucking filtration, filtrate is transferred PH2 with hydrochloric acid, and 55 ℃ are incubated 6 hours, the tipping supernatant, sucking filtration, precipitation washes with water to PH3～4, vacuum drying gets the Herba Erigerontis total flavones extract.
8. as containing the composite preparation of orientin and isorientin as described in the claim 6, it is characterized in that:
Wherein said step 3) is: orientin, isorientin extract and Herba Erigerontis total flavones extract are merged, add 1800 milliliters of waters for injection, stirring makes molten, it is an amount of to add glycerol again, mixing is transferred PH6.8-7.8 with saturated sodium carbonate, adds water for injection to 10000 milliliter, mixing, filter filtrate sterile filling, every 10ml with 0.45um and 0.22um microporous filter membrane, sterilized 60 minutes down, promptly get 1000 injection for 105 ℃.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424066A (en) * | 2002-12-19 | 2003-06-18 | 姚茂荣 | Chinese medical preparation for treating coronary disease and angina pectoris and preparation thereof |
| CN1785263A (en) * | 2005-12-09 | 2006-06-14 | 贵州益佰制药股份有限公司 | Quality control method of compound polygonium oriental preparation |
| CN1895367A (en) * | 2006-04-18 | 2007-01-17 | 贵州益佰制药股份有限公司 | Chinese-medicinal preparation for treating coronary heart disease and angina cordis and its preparation |
| CN101306091A (en) * | 2008-07-04 | 2008-11-19 | 贵州益佰制药股份有限公司 | Use of prince feather and fleabane combination in preparing medicament for treating kidney disease |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424066A (en) * | 2002-12-19 | 2003-06-18 | 姚茂荣 | Chinese medical preparation for treating coronary disease and angina pectoris and preparation thereof |
| CN1785263A (en) * | 2005-12-09 | 2006-06-14 | 贵州益佰制药股份有限公司 | Quality control method of compound polygonium oriental preparation |
| CN1895367A (en) * | 2006-04-18 | 2007-01-17 | 贵州益佰制药股份有限公司 | Chinese-medicinal preparation for treating coronary heart disease and angina cordis and its preparation |
| CN101306091A (en) * | 2008-07-04 | 2008-11-19 | 贵州益佰制药股份有限公司 | Use of prince feather and fleabane combination in preparing medicament for treating kidney disease |
Non-Patent Citations (2)
| Title |
|---|
| 兰燕宇等.注射用复方荭草(冻干粉针)指纹图谱研究.《中国中药杂志》.2005,第30卷(第6期), * |
| 吴莹等.注射用复方荭草冻干粉针中野黄芩苷的含量测定.《中国药业》.2005,第14卷(第7期), * |
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