CN101011550B - Medicinal composition for relieving stagnation, promoting circulation of qi and relieving pain, and its preparing process - Google Patents

Medicinal composition for relieving stagnation, promoting circulation of qi and relieving pain, and its preparing process Download PDF

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CN101011550B
CN101011550B CN2007100483420A CN200710048342A CN101011550B CN 101011550 B CN101011550 B CN 101011550B CN 2007100483420 A CN2007100483420 A CN 2007100483420A CN 200710048342 A CN200710048342 A CN 200710048342A CN 101011550 B CN101011550 B CN 101011550B
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李明劲
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Li Mingjin
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CHENGDU XICHEN PHARMACEUTICAL Co Ltd
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Abstract

The invention discloses a pharmaceutical composition for promoting circulation of qi and relieving pain and its preparing process, wherein the preparing process comprises the steps of weighing raw materials, disintegrating, immersing with 60-80% v/v ethanol, displacing and extracting, concentrating the percolation liquid to obtain concrete, disintegrating cape jasmine, immersing with 50-70% v/v ethanol, extracting through displacing, concentrating the percolation liquid to obtain concrete, disintegrating pomegranate bark and grilling, filtering to obtain filtrate, concentrating to obtain concrete, mixing the super fines, fines and fluid extract to obtain the medicinal composition.

Description

Pharmaceutical composition of a kind of relieving stagnation, promoting circulation of qi and relieving pain and preparation method thereof
Technical field
The present invention relates to pharmaceutical composition of a kind of relieving stagnation, promoting circulation of qi and relieving pain and preparation method thereof, particularly, relating to the natural drug is the medicine of feedstock production, belongs to field of medicaments.
Background technology
Mongols's proved recipe " the Six-element Radix Aucklandiae looses " records in 2005 editions one one 401 pages of the Pharmacopoeias of the People's Republic of China, and writing out a prescription is Radix Aucklandiae 200g, Fructus Gardeniae 150g, Pericarpium Granati 100g, Fructus Piperis Longi 70g, Fructus Amomi Rotundus 70g, Flos Rhododendri Mollis 100g; Method for making is ground into fine powder for getting crude drug, sieves, and mixing, promptly.But relieving stagnation, promoting circulation of qi and relieving pain is used for coldheat complex.Gastral cavilty feeling of fullness pain in the stagnation of QI due to Jiao, acid regurgitation and epigastric upset, belch abdominal distention, stomachache, stool are not well.
At present, take the rapid-action advantage in clothes back though the Six-element Radix Aucklandiae looses as powder, its divided dose is inaccurate, inconvenience when taking, and have the defective of mouthfeel discomfort.The Six-element Radix Aucklandiae capsule that Chengdu Xichen Pharmaceutical Co., Ltd. produces is encapsulated for directly getting powder, though capsule has solved the problem of divided dose, but the capsule taking dose after loading is big, need take 4~6 at every turn, every 0.42g, once take about 1.7~2.5g, and the capsule prolonged disintegration, the drug effect performance is not rapid.Above-mentioned two kinds of dosage forms all exist in the processing technology quality standard controlling index low, detect data and wait shortcomings such as influencing quality less.
Chinese patent 03135319.3, a kind of dissipating depression of QI circulation of qi promoting and analgesic medicine, disclosing with the Radix Aucklandiae, Fructus Gardeniae, Punica granatum L., Flos Rhododendri Mollis, Fructus Amomi Rotundus, Fructus Piperis Longi is the drop pill that feedstock production forms.Its preparation method is that the Radix Aucklandiae, Fructus Amomi Rotundus, Fructus Piperis Longi extract volatile ingredient with steam distillation, and distillate device is in addition preserved; The Radix Aucklandiae, Fructus Amomi Rotundus, Fructus Piperis Longi three's medicinal residues mix with Fructus Gardeniae, Punica granatum L., Flos Rhododendri Mollis, carry out percolation extraction or heating extraction or immersion with 0%~100% ethanol or ethyl acetate and extract or use water boiling and extraction, collect extracting solution, reclaim solvent, or mix with described distillate, be condensed into thick extractum; Thick extractum and volatile ingredient mixing join in the drop pill substrate of molten condition, and mix homogeneously obtains waiting to drip the medicinal liquid of making; Medicinal liquid is made drop pill in following of the condition that keeps 60~100 ℃ of steady temperatures, through cooling, is drying to obtain.Beneficial effect: simplify technology, reduced cost, improved medicine stability, and taking convenience, the medicine disintegrate is rapid, and onset is very fast.
Chinese patent 200310110569.5, the preparation method that Six-element Radix Aucklandiae capsule is new and the preparation of deriving, disclosing with the Radix Aucklandiae, Fructus Gardeniae, Punica granatum L., Flos Rhododendri Mollis, Fructus Amomi Rotundus, Fructus Piperis Longi is the drop pill capsule that feedstock production forms.Its preparation method is broken into coarse powder to extract volatile oil standby for getting the Radix Aucklandiae, Fructus Amomi Rotundus, Fructus Piperis Longi mixed powder; The medicinal residues of the Radix Aucklandiae, Fructus Amomi Rotundus, Fructus Piperis Longi and the coarse powder of Flos Rhododendri Mollis add 70~90% alcohol reflux, and merge extractive liquid, reclaims ethanol, and it is standby to get the ethanol extraction concentrated solution; Fructus Gardeniae, Punica granatum L. coarse powder decoct with water again, merge decoction liquor, filter, and the clear liquid thin film concentration adds above-mentioned ethanol extraction concentrated solution to the concentrated solution of relative density 1.05~1.10 (20~60 ℃), and mixing, drying, collection dried cream powder are standby; Getting above-mentioned volatile oil adds an amount of cyclodextrin to prepare clathrate standby; Get above-mentioned dried cream powder, cyclodextrin of volatile oil clathrate and appropriate amount of auxiliary materials mixing encapsulated/system micropill, drying, encapsulated, quality inspection, the packing, promptly; Or get the Radix Aucklandiae, Fructus Amomi Rotundus, Fructus Piperis Longi mixed powder and be broken into coarse powder to extract volatile oil standby; The coarse powder of medicinal residues and Punica granatum L., Fructus Gardeniae, Flos Rhododendri Mollis decocts with water, and the aqueous solution after merging decoction liquor and carrying oil is mixed, filters and removes precipitation, gets the concentrated solution of clear liquid thin film concentration to relative density 1.05~1.10 (20~60 ℃), and is dry, to collect dried cream powder standby; Getting above-mentioned volatile oil adds an amount of cyclodextrin to make clathrate standby; Get above-mentioned dried cream powder and add above-mentioned cyclodextrin of volatile oil clathrate and appropriate amount of auxiliary materials mixing, encapsulated, quality inspection, packing, promptly.This capsule dosage form consumption more in the past is reduced to 1/3 of former dose, carries taking convenience.
Chinese patent 03118942.3, Six-element Radix Aucklandiae granule and preparation method disclose four kinds of extracting method, and one is that the Radix Aucklandiae, Fructus Amomi Rotundus, Fructus Piperis Longi are carried volatile oil, and medicinal residues and Fructus Gardeniae, Punica granatum L., Flos Rhododendri Mollis decoct with water; It two beats fine powder for Fructus Piperis Longi, Flos Rhododendri Mollis, and the Radix Aucklandiae, Fructus Amomi Rotundus are carried volatile oil, and medicinal residues and Fructus Gardeniae, Punica granatum L. decoct with water; It three beats fine powder for Fructus Amomi Rotundus, Fructus Piperis Longi, Flos Rhododendri Mollis, and the Radix Aucklandiae is carried volatile oil, and medicinal residues and Fructus Gardeniae, Punica granatum L. decoct with water; It four beats fine powder for the Six-element raw material.Be prepared into granule through conventional method.Wherein need be ground into the medical material of fine powder in the technology and can routine be ground into 80~160 purpose fine powders or superfine powder is broken into 200~300 purpose fine powders.This invention granule has improvement to reservation and stable volatile ingredient, overcomes the inaccurate defective of powder divided dose, has kept onset advantage rapidly.
Summary of the invention
Technical problem to be solved by this invention provides a kind of new preparation method with pharmaceutical composition of relieving stagnation, promoting circulation of qi and relieving pain, particularly, provides Mongolian proved recipe " the Six-element Radix Aucklandiae looses " new extraction process.
Preparation method provided by the invention, it comprises the steps:
A, take by weighing the raw material Radix Aucklandiae, Fructus Piperis Longi, Flos Rhododendri Mollis, Fructus Amomi Rotundus, Fructus Gardeniae, Pericarpium Granati;
" the Six-element Radix Aucklandiae looses " according to 2005 editions 401 pages of records of the Pharmacopoeia of the People's Republic of China takes by weighing 200 parts of the raw material consumption Radix Aucklandiae, 150 parts of Fructus Gardeniaes, 100 parts of Pericarpium Granatis, 70 parts of Fructus Piperis Longi, 70 parts in Fructus Amomi Rotundus, 100 parts of Flos Rhododendri Mollis;
B, 1/3 amount of getting the raw material Radix Aucklandiae, Fructus Piperis Longi, that nutmeg is broken into micropowder is standby;
C, get the raw material Flos Rhododendri Mollis and be crushed to 100 mesh sieves;
D, 2/3 amount of getting the raw material Radix Aucklandiae were pulverized, with 60~80%v/v soak with ethanol 24 hours; The percolation post of after the immersion medical material and soak being packed into, 60~80%v/v ethanol when percolation adds, the percolate flow velocity is 4~6ml/ minute kg medical material, collects the ethanol percolation liquid of 11~12 times of medical material weight, concentrate fluid extract;
Employed immersion ethanol and percolation concentration of ethanol are 70%v/v among the preferred steps d.
E, get the raw material Fructus Gardeniae, pulverize, with 50~70%v/v soak with ethanol 24 hours; The percolation post of after the immersion medical material and soak being packed into, 50~70%v/v ethanol when percolation adds, the percolate flow velocity is 4~8ml/ minute kg medical material, collects the ethanol percolation liquid of 11~12 times of medical material weight, concentrate fluid extract;
Employed immersion ethanol and percolation concentration of ethanol are 70%v/v among the preferred steps e.
F, get the raw material Pericarpium Granati, pulverize, decoct with water, filter filtrate, concentrate fluid extract;
G, get step b gained micropowder, step c gained fine powder, steps d, e, f gained fluid extract mix, and promptly get pharmaceutical composition.
Wherein, preferred 70% ethanol of employed immersion ethanol and percolation concentration of ethanol in the steps d.
Alcoholic acid dense preferred 70% ethanol of employed immersion ethanol and percolation among the step e.
According to the Chinese medicine rationale, the Radix Aucklandiae is the principal agent in the raw material, and amount is big, and medical material multifilament matter, as not dealing with whole pulverizing, tabletting when being unfavorable for preparation.Take partly superfine grinding, the technology extracted of percolation partly, to reduce dose, tabletting when being beneficial to preparation, partly percolation extracts the volatile component that can effectively keep again in the Radix Aucklandiae simultaneously, guarantees curative effect.
Second technical problem to be solved by this invention provides the pharmaceutical composition of preparation method gained of the present invention.
Pharmaceutical composition of the present invention be with the preparation of the inventive method of effective dose pharmaceutical composition be active component, add the preparation of acceptable accessories or complementary composition and preparation.Wherein every gram pharmaceutical composition contains costunolide and is not less than 1.0mg, jasminoidin and is not less than the quality standard that 6.0mg, piperine are not less than 2.5mg.It is 2.02mg, jasminoidin 8.52mg, piperine 3.53mg that the present invention specifically detects content determination of costunolide.
Wherein, preparation is an oral formulations, particularly, is tablet, capsule, granule, pill or oral liquid.
In the inventive method with 03118942.3,200310110569.5,03135319.3 the method for three patent disclosures is compared, preparation method of the present invention is extracted and the combination of modern micronizing technology with traditional Chinese medicine percolation, the principal agent Radix Aucklandiae has been taked partly to pulverize the partly method of percolation extraction, both reduce dose, guaranteed curative effect again; Simultaneously, Flos Rhododendri Mollis is not adopted the method for extraction, because of it belongs to malicious drastic material, active ingredient is still very not clear, so take safe breaking method.Three kinds of methods of this method and other are compared, have technical maturity, simple, consume low advantage.
The specific embodiment
Below beneficial effect by craft screening test and assay evidence preparation method of the present invention and pharmaceutical composition.
One, Radix Aucklandiae extraction process screening test
1, the mensuration of volatile oil: press one one 2005 editions appendix XD methods of Chinese Pharmacopoeia and measure (57 pages of appendix).
Contain not regulation content of volatile oil 0.5ml/100g pharmacopeia in the Radix Aucklandiae, document (Xu Hui Chin PharmJ.2006 vo141.16.1214 page or leaf) adopts steam distillation, and 12h gets volatile oil, yield 0.49%, and wherein do not detect costunolide and dehydrogenation costunolide.
2, water boiling and extraction: the method for decocting Chinese medicine routinely, get Radix Aucklandiae 100g coarse powder, add 10 times of amounts of water and decoct, little boiling 1.5 hours filters; Medicinal residues add 8 times of amounts of water, decoct 1 hour, filter, and merging filtrate, concentrating under reduced pressure is lower than 60 ℃, dried cream yield 30%, wherein costunolide 0.02%, and as index components, decocting boils with the costunolide composition, is unfavorable for the enrichment of this composition.
3, different concentration ethanol is extracted: the Radix Aucklandiae contains volatile ingredient, extracts in the concentration process and should avoid high temperature as far as possible, the first-selected normal temperature percolation of inventor, the way of cryoconcentration.Percolation speed adopts conventional 5ml/Kgmin.
The investigation of percolate consumption: get Radix Aucklandiae 200g coarse powder, 70% soak with ethanol 24 hours, percolation, one bottle of flow velocity 5ml/Kg nin250ml collects percolate, changes bottle at every turn and gets 10ml and be concentrated into driedly, adds chloroform 10ml, and dissolving moves in the 10ml measuring bottle to scale.Get 5ul and carry out thin layer discriminating (2005 editions 42 pages of Radix Aucklandiae of the Pharmacopoeia of the People's Republic of China are differentiated) by official method.The costunolide reference substance, each 0.5mg/ml point of dehydrogenation costunolide reference substance is the silica gel g thin-layer plate of binding agent in same sodium carboxymethyl cellulose.With chloroform-cyclohexane extraction (5: 1) is developing solvent, launches, and takes out, and dries, and sprays 1% vanillin sulfuric acid solution, heating.
The result: 1-7 part speckle is obvious, and 8-10 part speckle color and luster is gradually shallow, cannot see speckle for the 10th part, promptly about 2250~2500ml, and percolate does not have the costunolide constituents.Be that the percolation cumulative volume is controlled about 12 times of amounts.
The comparison of different concentration ethanol
Get Radix Aucklandiae 200g coarse powder, with 30%, 50%, 70%, 90% ethanol.2 times of amounts were soaked 24 hours, 10 times of amount percolation, and flow velocity 5ml/kg/min collects percolate, concentrating under reduced pressure.Be lower than 60 ℃, it is heavier to get dry extract.HPLC measures the costunolide experimental result and sees Table 1:
Table 1HPLC measures costunolide
Figure G200710048342020070209D000041
Can learn that by table 1 different concentration ethanol is extracted, with 70% ethanol extraction, receive content determination of costunolide the highest, conversion ratio is also the highest.
Learn from experimental data: the index components costunolide.Dehydrogenation costunolide content in volatile oil is not high, and it is easy to be extracted by Diluted Alcohol, is difficult for by water extraction.
The repeated trials of 70% ethanol percolate extraction: three times repeated trials the results are shown in Table 2:
Table 270% ethanol percolate extraction repeated trials
With rare alcohol extraction Radix Aucklandiae, but the enrichment index components, but the composition conversion ratio in the extract is lower, so reserve part medicated powder does not extract, the one-tenth dosis refracta in the pharmaceutical composition of the present invention is reduced.
Two, Fructus Gardeniae extraction process screening test
Active component is iridoids and glycoside and Gardenia Yellow in the Fructus Gardeniae, relevant its research and development, Ni Huiyan etc. also write one piece of summary (CHINA JOURNAL OF CHINESE MATERIA MEDICA 31-7-538 in 2006) in the time approximately identical with inventor's research work, Hu Zhen has also done " jasminoidin extraction process and HPLC analyze in the Fructus Gardeniae " (Chinese patent medicine was rolled up 336 pages of 3 phases in 2006 38), propose to measure 80% alcohol reflux 1 time, can obtain higher extraction ratio with 5 times.
1. hot water extraction test
Get Fructus Gardeniae 200g, coarse pulverization adds 10 times of amounts of water, decocts, and keeps little and boils 1.5 hours, filters, and residue adds 10 times of amounts of water, decocts 1 hour, filters merging filtrate, concentrating under reduced pressure.(temperature≤60 ℃)
2. different concentration ethanol is extracted test
Get Fructus Gardeniae 200g, coarse pulverization adds 2 times of amounts of different concentration ethanol (30%, 50%, 70%, 90%) and soaked 24 hours, oozes slag (10 times of amounts), and flow velocity 3~5ml/kg/min collects percolate, concentrating under reduced pressure.(temperature≤60 ℃) the results are shown in following table 3:
Table 3 different concentration ethanol is extracted test
Figure G200710048342020070209D000051
Can learn by table 3, use 70% ethanol extraction, receive jasminoidin content the highest.
3. the repeated trials that extracts of Fructus Gardeniae: the results are shown in Table 4 with batch three repeated trials of medical material:
The repeated trials that table 4 Fructus Gardeniae is extracted
Figure G200710048342020070209D000052
4. discuss:
Hu Zhen has mentioned the selection of extracting method, the selection result of the test of different solvents, jasminoidin content (%) in " jasminoidin extraction process and HPLC analyze in the Fructus Gardeniae " literary composition.
Normal hexane 1.62 ether 1.7460% alcohol 2.29
Petroleum ether 1.52 methanol 2.3470% alcohol 2.32
Chloroform 1.38 acetone 1.4280% alcohol 2.34
Ethyl acetate 1.22 ethanol 2.27
The result shows: 11 kinds of different solvents extract, 80%, 70% ethanol extraction, and the content of jasminoidin is the highest in the extract of gained.
The document is the more different extracting method of ratio of solvent with identical solvent (80% ethanol of 5 times of amounts) again simultaneously, comprises infusion method, ultrasonic method, and percolation, circumfluence method and soxhlet extraction, jasminoidin content sees Table 5 in the extract.Hu Zhen was return time 30 minutes, 60 minutes, 90 minutes in addition, and jasminoidin content is respectively 2.43,2.51,2.37 pairs of return times and makes orthogonal test in the extract, 3 factors, 3 levels, 80% alcohol heating reflux 1 time, and each 1 hour is optimum condition.
Table 5 extracting method is selected result of the test
Report to Hu Zhen: 80% ethanol and 70% ethanol, jasminoidin content only differ from 0.02% (2/10000ths).Analytical error also may cause this difference, the difference of the extracting method that is not enough to illustrate that preparation method of the present invention and Hu Zhen provide.
Three, Pericarpium Granati extraction process screening test
Reported in literature Pericarpium Granati decoct, alkaloids are anthelmintic active component, and it also contains tannin, tannic acid, gallic acid, belulinic acid Betulinic acid, ursolic acid etc.Suit to use hot water extraction, but will prevent long-time high temperature heating, the pectin toughness helps extractum is granulated as binding agent in the peel in addition.The pharmacopeia regulation has the mensuration of content of tannin, and the inventor adopts version pharmacopeia tannin assay method (hide powder method) in 2000.Measure the tannin total content and estimate extracting method.
1. hot extracting method:
Get Pericarpium Granati 100g, coarse pulverization adds 10 times of amounts of water, soaks 30 minutes, decocts, and keeps little and boiled 1 hour, filters.Filtering residue adds 8 times of amounts of water, decocts, and keeps little and boiled 1 hour, filters, and merges filtrate twice, the concentrating under reduced pressure drying.(temperature≤60 ℃)
2. content of tannin is measured: 63 pages of content of tannin assay methods of appendix of version pharmacopeia in 2000
The material test sample powder (cross No. three sieve) an amount of (containing the about 1g of tannin) of getting it filled accurately claims surely, puts in the conical flask, adds water 150ml, and heating is 30 minutes in water-bath, after the cooling, move in the 250ml measuring bottle, and filtration, filtrate is as need testing solution.The mensuration precision of total water-soluble portion is measured need testing solution 25ml, evaporate to dryness, and residue was in 105 ℃ of dryings 3 hours, and (T weighs 1).
Do not measure need testing solution 100ml with the mensuration precision of the bonded water-soluble portion of corium farinosum, add corium farinosum (dry product 6g), jolting 15 minutes filters, and precision is measured filtrate 25ml, evaporate to dryness, and residue was in 105 ℃ of dryings 3 hours, and (T weighs 2).
The mensuration precision of corium farinosum water-soluble portion is measured water supply 100ml, adds corium farinosum (dry product 6g), and jolting 15 minutes filters, and precision is measured 25ml, evaporate to dryness, and residue was in 105 ℃ of dryings 3 hours, and (T weighs 0).Be calculated as follows the content (%) of tannin:
Figure G200710048342020070209D000061
W is sampling amount (dry product) g in the formula.
3. Pericarpium Granati extracts repeated trials: the results are shown in Table 6 with batch three repeated trials of medical material:
Table 6 Pericarpium Granati extracts repeated trials
Figure G200710048342020070209D000062
Remarks: content of tannin 23.74% in the Pericarpium Granati crude drug.
Four, Fructus Amomi Rotundus extraction process screening test
The Fructus Amomi Rotundus pharmacopeia stipulates that its former Fructus Amomi Rotundus core volatile oil content is not less than 5 ‰, and Indonesia's Semen Vignae Cylindricae KOUREN volatile oil content is not less than 4.0% (ml/g), and Fructus Amomi Rotundus has fragrance and is good for the stomach, the function of gallbladder promoting function is obvious, and it can also promote gastric secretion, excited enterokinesia, drive away the enteral pneumatosis, suppress enteral abnormal fermentation.But have yet and think and only consider that its volatile ingredient is incomplete for its effective ingredient, active component is very not clear and definite, and the inventor did research to be had:
(1) determination of volatile oil: medical material being measured, do not adopted Fructus Amomi Rotundus core to measure, is lower so contain, and does not reach standards of pharmacopoeia.70g Fructus Amomi Rotundus medical material, coarse powder adds water 560ml, little boiling 3 hours collected volatile oil 0.2ml, the secondary redistillation adds water 560ml, no longer increase to volatile oil, volatile oil 0.08ml.
(2) after volatile oil extracts, filter, medicinal residues continue water and decoct, and collecting decoction filters, and filtrate merges, and concentrates, and the 8.0g that gets dry extract, yield are 11.4%.
Because the index composition is indeterminate, have to abandon extracting, still to pulverize, micropowder is used as medicine, and is better than extracting.In view of Fructus Amomi Rotundus when using water as solution and extract, its yield is low, the volatilization oil mass is not easy to collect less, so abandon it is done to extract processing.
Five, Fructus Piperis Longi extraction process screening test
Fructus Piperis Longi contains volatile oil, lactams such as piperine, alkaloid, lignan component.Volatile oil has sedation, petroleum ether, and ethyl acetate extraction can prolong the sodium phenobarbital mouse sleep time; Ethanol extraction has obvious anti-gastric-ulcer effect, also has gastric acid inhibitory secretory action etc., and index components is a piperine, pharmacopeia must not stipulate and is less than 2.5%, it is difficult to indicate the quality of distinguishing extraction process owing to also very not definite to its active component at present, temporarily keeps medicated powder and is used as medicine.
Determination of volatile oil: get Fructus Piperis Longi 70g, coarse pulverization adds drinking water 560ml, soaked 30 minutes, and decocted, and kept little 3 hours, collect volatile oil 0.15ml, leave standstill cooled and filtered, get filtrate, residue adds drinking water 560ml, and decocting and keeping little does not increase (shared 2 hours) to volatile oil, volatile oil 0.06ml, cooling is filtered.Merge 2 times filtrate, concentrating under reduced pressure (60 ℃ of temperature) gets dry extract 10.6g.Pharmacopeia to the mensuration of its volatile oil, not can not find reference numerical value.
In view of Fructus Piperis Longi when using water as solution and extract, its yield is low, the volatilization oil mass is not easy to collect less, so abandon it is done the water extraction processing.
Six, Flos Rhododendri Mollis extraction process screening test
Flos Rhododendri Mollis is strong analgesic, is again the toxicity medical material, but its accurate active chemical components still not fully aware of at present adopts former powder formale amount and method for making, promptly is ground into fine powder, does not do to extract and handles.
In the inventive method with 03118942.3,200310110569.5,03135319.3 the method for three patent disclosures is compared, preparation method of the present invention is extracted and the combination of modern micronizing technology with traditional Chinese medicine percolation, the principal agent Radix Aucklandiae has been taked partly to pulverize the partly method of percolation extraction, both reduce dose, guaranteed curative effect again; Simultaneously, Flos Rhododendri Mollis is not adopted the method for extraction, because of it belongs to malicious drastic material, active ingredient is still very not clear, so take safe breaking method.Three kinds of methods of this method and other are compared, have technical maturity, simple, consume low advantage.

Claims (6)

1. the preparation of drug combination method of relieving stagnation, promoting circulation of qi and relieving pain comprises the steps:
A, take by weighing raw material: 200 parts of the Radix Aucklandiae, 150 parts of Fructus Gardeniaes, 100 parts of Pericarpium Granatis, 70 parts of Fructus Piperis Longi, 70 parts in Fructus Amomi Rotundus, 100 parts of Flos Rhododendri Mollis according to the following weight proportioning;
B, 1/3 amount of getting the raw material Radix Aucklandiae are with Fructus Piperis Longi, that nutmeg is broken into micropowder is standby;
C, get the raw material Flos Rhododendri Mollis and be crushed to 100 mesh sieves;
D, 2/3 amount of getting the raw material Radix Aucklandiae were pulverized, with 60~80%v/v soak with ethanol 24 hours; After the immersion medical material gone into the percolation post, 60~80%v/v ethanol when percolation adds, the percolation flow velocity is 4~6ml/ minute kg medical material, collects the ethanol percolation liquid of 11~12 times of medical material weight, concentrate fluid extract;
E, get the raw material Fructus Gardeniae, pulverize, with 50~70%v/v soak with ethanol 24 hours; The percolation post of after the immersion medical material and soak being packed into, 50~70%v/v ethanol when percolation adds, the percolate flow velocity is 4~8ml/ minute kg medical material, collects the ethanol percolation liquid of 11~12 times of medical material weight, concentrate fluid extract;
F, get the raw material Pericarpium Granati, pulverize, decoct with water, filter filtrate, concentrate fluid extract;
G, get step b gained micropowder, step c gained fine powder, steps d, e, f gained fluid extract mix, and promptly get pharmaceutical composition.
2. preparation method according to claim 1 is characterized in that: employed immersion ethanol and percolation concentration of ethanol are 70%v/v in the described steps d.
3. preparation method according to claim 1 is characterized in that: employed immersion ethanol and percolation concentration of ethanol are 70%v/v among the described step e.
4. the pharmaceutical composition of a claim 1 preparation gained is characterized in that: be with claim 1 preparation of effective dose pharmaceutical composition be active component, add the acceptable accessories preparation and preparation.
5. pharmaceutical composition according to claim 4 is characterized in that: described preparation is an oral formulations.
6. pharmaceutical composition according to claim 5 is characterized in that: described oral formulations is tablet, capsule, granule, pill or oral liquid.
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中华人民共和国卫生部药典委员会.《六味木香胶囊》.《卫生部颁药品标准 新药转正标准 第29册》.2001,16. *
杨金团.《六味木香胶囊的药理作用及临床应用》.《中国民族医药杂志》.2005,(第6期),22-23. *

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