CN102397267A - Method for preparing sinomenine hydrochloride cataplasma - Google Patents
Method for preparing sinomenine hydrochloride cataplasma Download PDFInfo
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Abstract
The invention provides a method for preparing a sinomenine hydrochloride cataplasma. The method has the advantages that: sinomenine hydrochloride is prepared through percolation; the operation is simple; in an extraction process, heating is not required and cooling is performed; the yield is high; mother liquid is simply treated; and the method is safe and reliable, is low in pollution, and plays an active role inof protecting environment.
Description
Technical field
The present invention relates to a kind of method for preparing of sinomenine hydrochloride cataplasma, be specifically related to a kind of percolation and extract the method that effective ingredient sinomenine hydrochloride in the Caulis Sinomenii is processed cataplasma.
Background technology
Caulis Sinomenii is a conventional Chinese medicine; Dry rattan for menispermaceous plants Sinomenium acutum and hair Sinomenium acutum; Just on the books in Compendium of Material Medica, record in Pharmacopoeia of the People's Republic of China version in 2010 at present, have dispel the wind, the effect of the meridian dredging, diuresis; Be used to treat rheumatic arthralgia, arthroncus, paralysis pruritus, also have effects such as anti-arrhythmia and blood pressure lowering.
Main component is an alkaloid in the Caulis Sinomenii; The composition of having found at present has sinomenine (Sinomenine); Isosinomenine (Igoginomenine), magnificent sinomenine (SinoAcutine), short Sinomenium acutum time alkali (Acutumidine); Point sinomenine (Sinaetine) and disinomenine (Diginomenine), ethyl sinomenine (ethylsinomenine), tetrahydrochysene epiberberine (sinactine), tetrahydrochysene epiberberine, Caulis menispermi ripple phenol alkali, bianfugenine, Tetrahydropalmatine etc.
Sinomenine (Sinomenine) is a kind of alkaloid monomer that extracts in the Caulis Sinomenii, is the main effective ingredient of Caulis Sinomenii performance analgesia, antiinflammatory action, from Japanese Caulis Sinomenii, is separated obtaining the earliest by Ishiwari etc.The sixties in 20th century, Chinese scholar Zhu Renhong also found sinomenine from homemade Caulis Sinomenii.Its hydrochlorate preparation commonly used clinically such as ZHENGQINGFENGTONGNING PIAN, ZHENGQINGFENGTONGNING slow releasing tablet, ZHENGQINGFENGTONGNING injection are used to treat rheumatic, rheumatoid arthritis, and treatment ankylosing spondylitis, arrhythmia etc. are evident in efficacy.
At present the commercial production sinomenine hydrochloride adopts the alkalization water extraction process more, and it is for adding entry and a certain amount of Calx in Caulis Sinomenii, alkalization a period of time, add a certain amount of technical benzene then, reflux, extract, in water-bath, last acidify, leave standstill, crystallize.
Document has report to introduce the extraction and the purification process of sinomenine at present, and Caulis Sinomenii dilute sulfuric acid percolate is with lime water adjust pH 9; Benzene carries out counter-current extraction at 50 ℃, and benzene extraction liquid carries out the extraction of regurgitation stream, activated carbon decolorizing with 1% hydrochloric acid; Recrystallization is carried out in crystallization in hot water, get pure article.(Chen Yukun " extracting technique of Chinese medicine ", 1992)
This several method all uses the very big benzene of toxicity as extracting solvent; Benzene is I class toxic solvent; Murder by poisoning to human body is main with blood system and neurasthenia's disease crowd, shows as blood leukocytes, platelet and erythrocytopenia, dizziness, headache, hypomnesis, insomnia etc.Aplastic anemia can take place in severe patient, even leukemia, death, and is disabled at pharmaceutical industry.And the recovery of benzene is comparatively cumbersome, and the discharging difficulty reaches environmental requirement.Thereby in Chinese medicine extraction, replace the key that the raw material that contains benzene is the prevention benzolism with the raw material that does not contain benzene.
Summary of the invention
The invention provides a kind of method for preparing of sinomenine hydrochloride cataplasma.
Goal of the invention realizes that through following technical scheme the method for preparing of sinomenine hydrochloride cataplasma of the present invention comprises the steps:
The preparation of step 1, sinomenine hydrochloride:
A, preparation sinomenine hydrochloride bullion
1, extract: Caulis Sinomenii coarse powder 100～1000 weight portions, with 0.1～1mol/L HCl moistening of 60～1000 parts by volume 0.5～8 hour, adorn percolator; Adding 0.1～1mol/L HCl again makes liquid level cover medicated powder 2cm; Flood after 6～48 hours, begin percolation, stop percolation after 6～24 hours by the speed of 2～6ml/min; Get percolate, subsequent use;
2, extraction: above-mentioned percolate is added lime cream transfer pH to 10.5～12.0, filter, filtrating adds hydrochloric acid and transfers pH to 7.0～9.5, with chloroform extraction 2～5 times; Combined chloroform layer water is washed till neutrality, adds the anhydrous Na2SO4 dehydration of 3%～6% times of weight, and concentrating under reduced pressure reclaims chloroform;
3, crystallization: concentrated solution splashes into 6mol/L HCl and transfers pH to 2～4, and be stirred to the come-up solids and disperse, cold preservation, sucking filtration discards filtrating, and 60 ℃～70 ℃ oven dry filter cakes get yellow sinomenine hydrochloride bullion;
B, sinomenine hydrochloride process for refining
Get sinomenine hydrochloride bullion 5～10 weight portions,, add the active carbon of 4% times of weight with 10～95% ethanol or the dissolving extremely fully of purified water reflux of 30～120 parts by volume; Insulation refluxed 10～30 minutes, filtered while hot, and filtrating concentrates; Cooling, crystallize; Filter, it is colourless to filtrating that the ethanol with 95% cleans filter cake, gets sinomenine hydrochloride;
Take by weighing sodium polyacrylate (NP-700), polyvinylpyrrolidone (K-30), Kaolin, glycosides hydroxyl aluminum, sinomenine hydrochloride, mix homogeneously joins in the glycerol, stirs to obtain the A phase; Oleum menthae and sinomenine hydrochloride are added in the distilled water, obtain the B phase; Take by weighing tartaric acid, obtain the C phase with dissolving in the distilled water.
With A mutually with B mix homogeneously mutually, to wherein slowly stirring adding C phase, stirred 10～20 minutes, obtain the thickness mastic; Mastic is evenly coated on the medical adhesive-bonded fabric, covered adherent layer, more than 18-36 hour, make mastic full cross-linked in 25-28 ℃, 40--60% damp condition held.Step 1 in the method for preparing of sinomenine hydrochloride cataplasma of the present invention can be preferably:
A, preparation sinomenine hydrochloride bullion
1, extract: Caulis Sinomenii coarse powder 500 weight portions, with the 0.5mol/L HCl moistening of 500 parts by volume 2 hours, adorn percolator; Add 0.5mol/L HCl again and make liquid level cover medicated powder 3cm, flood after 24 hours, begin percolation by the speed of 3ml/min; Stop percolation after 15 hours, get percolate, subsequent use;
2, extraction: above-mentioned percolate is added lime cream transfer pH to 11.6, filter, filtrating adds hydrochloric acid and transfers pH to 8, with chloroform extraction 4 times; Combined chloroform layer water is washed till neutrality, adds the anhydrous Na2SO4 dehydration of 3% times of weight, and concentrating under reduced pressure reclaims chloroform;
3, crystallization: concentrated solution splashes into 6mol/L HCl and transfers pH to 3, and be stirred to the come-up solids and disperse, cold preservation, sucking filtration discards filtrating, and 65 ℃ of oven dry filter cakes get yellow sinomenine hydrochloride bullion;
B, sinomenine hydrochloride process for refining
Get sinomenine hydrochloride bullion 7 weight portions, the concentration of using 60 parts by volume is 75% alcohol heating reflux dissolving extremely fully, adds the active carbon of 4% times of weight; Insulation refluxed 20 minutes, filtered while hot, and filtrating concentrates; Cooling, crystallize; Filter, it is colourless to filtrating that the ethanol with 95% cleans filter cake, gets sinomenine hydrochloride.
A, preparation sinomenine hydrochloride bullion
1, extract: Caulis Sinomenii coarse powder 400 weight portions, with the 0.3mol/L HCl moistening of 320 parts by volume 3.5 hours, adorn percolator; Add 0.3mol/L HCl again and make liquid level cover medicated powder 4cm, flood after 6 hours, begin percolation by the speed of 6ml/min; Stop percolation after 8 hours, get percolate, subsequent use;
2, extraction: above-mentioned percolate is added lime cream transfer pH to 11.3, filter, filtrating adds hydrochloric acid and transfers pH to 8.5, with chloroform extraction 2 times; Combined chloroform layer water is washed till neutrality, adds the anhydrous Na2SO4 dehydration of 5% times of weight, and concentrating under reduced pressure reclaims chloroform;
3, crystallization: concentrated solution splashes into 6mol/L HCl and transfers pH to 4, and be stirred to the come-up solids and disperse, cold preservation, sucking filtration discards filtrating, and 62 ℃ of oven dry filter cakes get yellow sinomenine hydrochloride bullion;
B, sinomenine hydrochloride process for refining
Get sinomenine hydrochloride bullion 10 weight portions,, add the active carbon of 4% times of weight with the 95% alcohol heating reflux dissolving extremely fully of 120 parts by volume; Insulation refluxed 25 minutes, filtered while hot, and filtrating concentrates; Cooling, crystallize; Filter, it is colourless to filtrating that the ethanol with 95% cleans filter cake, gets sinomenine hydrochloride.Step 1 in the method for preparing of sinomenine hydrochloride cataplasma of the present invention can also be preferably:
A, preparation sinomenine hydrochloride bullion
1, extract: Caulis Sinomenii coarse powder 200 weight portions, with the 0.2mol/L HCl moistening of 900 parts by volume 3.5 hours, adorn percolator; Adding 0.8mol/L HCl again makes liquid level cover medicated powder 4cm; Flood after 15 hours, begin percolation, stop percolation after 20 hours by the speed of 4ml/min; Get percolate, subsequent use;
2, extraction: above-mentioned percolate is added lime cream transfer pH to 11.3, filter, filtrating adds hydrochloric acid and transfers pH to 9, with chloroform extraction 2 times; Combined chloroform layer water is washed till neutrality, adds the anhydrous Na2SO4 dehydration of 5% times of weight, and concentrating under reduced pressure reclaims chloroform;
3, crystallization: concentrated solution splashes into 6mol/L HCl and transfers pH to 4, and be stirred to the come-up solids and disperse, cold preservation, sucking filtration discards filtrating, and 62 ℃ of oven dry filter cakes get yellow sinomenine hydrochloride bullion;
B, sinomenine hydrochloride process for refining
Get sinomenine hydrochloride bullion 8 weight portions,, add the active carbon of 4% times of weight with 50% ethanol or the dissolving extremely fully of purified water reflux of 12 parts by volume; Insulation refluxed 25 minutes, filtered while hot, and filtrating concentrates; Cooling, crystallize; Filter, it is colourless to filtrating that the ethanol with 95% cleans filter cake, gets sinomenine hydrochloride.
A, preparation sinomenine hydrochloride bullion
1, extract: Caulis Sinomenii coarse powder 800 weight portions, with the 0.8mol/L HCl moistening of 300 parts by volume 1 hour, adorn percolator; Add 0.2mol/L HCl again and make liquid level cover medicated powder 5cm, flood after 36 hours, begin percolation by the speed of 5ml/min; Stop percolation after 8 hours, get percolate, subsequent use;
2, extraction: above-mentioned percolate is added lime cream transfer pH to 11.3, filter, filtrating adds hydrochloric acid and transfers pH to 7, with chloroform extraction 5 times; Combined chloroform layer water is washed till neutrality, adds the anhydrous Na2SO4 dehydration of 6% times of weight, and concentrating under reduced pressure reclaims chloroform;
3, crystallization: concentrated solution splashes into 6mol/L HCl and transfers pH to 2, and be stirred to the come-up solids and disperse, cold preservation, sucking filtration discards filtrating, and 68 ℃ of oven dry filter cakes get yellow sinomenine hydrochloride bullion;
B, sinomenine hydrochloride process for refining
Get sinomenine hydrochloride bullion 6 weight portions,, add the active carbon of 4% times of weight with 80% ethanol or the dissolving extremely fully of purified water reflux of 40 parts by volume; Insulation refluxed 15 minutes, filtered while hot, and filtrating concentrates; Cooling, crystallize; Filter, it is colourless to filtrating that the ethanol with 95% cleans filter cake, gets sinomenine hydrochloride.
Take by weighing sodium polyacrylate (NP-700), polyvinylpyrrolidone (K-30), Kaolin,, glycosides hydroxyl aluminum, sinomenine hydrochloride, mix homogeneously joins in the glycerol, stirs to obtain the A phase; Transdermal enhancer Oleum menthae and sinomenine hydrochloride are added in the distilled water, obtain the B phase; Take by weighing tartaric acid, obtain the C phase with dissolved in distilled water; With A mutually with B mix homogeneously mutually, to wherein slowly stirring adding C phase, stirred 10～20 minutes, obtain the thickness mastic; Mastic is evenly coated on the medical adhesive-bonded fabric, covered adherent layer, cut into the certain specification size, more than 24 hours, make mastic full cross-linked in 27 ℃, 50% damp condition held.
The weight portion in the method for preparing of above-mentioned sinomenine hydrochloride cataplasma and the relation of parts by volume are the relation of g/ml.
The method for preparing of sinomenine hydrochloride cataplasma provided by the invention, advantage are wherein to have adopted percolation to prepare the step of sinomenine hydrochloride, and simple to operate, leaching process need not heat, and is cold treatment; Yield is high, and mother solution is handled simple; Safe and reliable, pollute lowly, environmental conservation is played a positive role.
Description of drawings
Accompanying drawing 1:0.1mol/L hydrochloric acid extraction 2,4,6,10,12,24,28,30, the Ultraluminescence thin layer collection of illustrative plates after 48 hours and colour developing thin layer collection of illustrative plates
Accompanying drawing 2:0.3mol/L hydrochloric acid extraction 2,4,6,10,12,24,28,30, the Ultraluminescence thin layer collection of illustrative plates after 48 hours and colour developing thin layer collection of illustrative plates
Accompanying drawing 3:0.7mol/L hydrochloric acid extraction 2,4,6,10,12,24,28,30, the colour developing thin layer collection of illustrative plates after 48 hours
Accompanying drawing 4:1.0mol/L hydrochloric acid extraction 2,4,6,10,12,24,28,30, the colour developing thin layer collection of illustrative plates after 48 hours
Accompanying drawing 5:0.1,0.3,0.7, the 1.0mol/L concentration hydrochloric acid extraction colour developing thin layer collection of illustrative plates after 12 hours
Accompanying drawing 6: the percolation time is 2,4,6,10,12,14 hours colour developing thin layer collection of illustrative plates
Accompanying drawing 7: it is 7,8,9,10 that aqueous alkali is transferred pH, 11 fluorescence and colour developing thin layer collection of illustrative plates
Accompanying drawing 8: with the extract fluorescence and the colour developing thin layer chromatography of chloroform extraction 1 time, 2 times, 3 times, 4 times
Accompanying drawing 9: percolate, aqueous alkali, weak lye, extract, elaboration, mother solution, elaboration fluorescence and colour developing thin layer chromatography
Accompanying drawing 10: sinomenine hydrochloride reference substance high-efficient liquid phase chromatogram
Accompanying drawing 11: the liquid chromatogram of sinomenine hydrochloride
Accompanying drawing 12: the thin-layer chromatogram of sinomenine hydrochloride, the 1st speckle are reference substance, and the 2nd, 3,4,5 speckles are respectively 4 samples of the present invention.
Following experimental example and embodiment are used to further specify but are not limited to the present invention.
Experimental example one: Caulis Sinomenii Study on extraction
1, test objective
Through this test, confirm the technological parameter of this extraction process, like dip time, percolation time, extraction times, pH regulator scope etc., optimize technology.
2, test material
2.1 raw material: the Caulis Sinomenii that the Baoji provides
2.2 instrument:
Percolator;
PHS-2F PH meter: go up Electronic Instruments Plant of Nereid section
ZF-2 type three is used ultraviolet device: go up Hai'an booth Electronic Instruments Plant
RE-52A Rotary Evaporators: Shanghai Yarong Biochemical Instrument Plant
SHB-3 recirculated water is used vacuum pump more: Zhengzhou Tu Fu instrument plant
2.3 reagent: the quartzy chemical company limited in hydrochloric acid Zhuzhou
The safe and sound fine chemistry industry of ammonia Changsha Industrial Co., Ltd.
Chloroform Chemical Reagent Co., Ltd., Sinopharm Group
Silica gel G: Qingdao Marine Chemical Co., Ltd.
Ca (OH) 2, Na2SO4, bismuth potassium iodide weak solution, ethanol etc.
2.4 detection method: colour developing thin layer chromatography
Thin layer chromatography condition: immobile phase, silica gel thin-layer plate; Developing solvent, methanol: water: ammonia=8: 1: 1 developers, bismuth potassium iodide weak solution; The point sample amount, 5ul.
3, method
3.1 concentration of hydrochloric acid and dip time are investigated
Take by weighing 4 parts of mistakes, 20 purpose Caulis Sinomenii coarse powder, every part of 50g is respectively charged in 4 100ml beakers; Prepare 0.1mol/L, 0.3mol/L, 0.7mol/L, 1.0mol/L hydrochloric acid; Added in 4 beakers moistening respectively 0.5 hour with the hydrochloric acid of the above-mentioned concentration of 40ml; In each beaker, add hydrochloric acid 50ml again with concentration, dipping, sampling in per 2 hours is taken a sample respectively 1 time.
Judgment basis:
1, by same concentration, different dip time sample is put in chronological order on same lamellae respectively, compared with the reference substance speckle, the maximum time point of principal spot is a dip time;
2, the sample of same time period, variable concentrations is put on same lamellae by the concentration order, the concentration point maximum with principal spot is optium concentration;
When 3, representing concentration result not have significant difference, show that then the hydrochloric acid of 0.1～1.0mol/L all is fit to this extraction as if 4.
3.2 the percolation time is investigated
The hydrochloric acid of getting 3.1 said definite concentration is as solvent; Cross 20 purpose sinomenine coarse powder 0.5 hour with 160ml moistening 200g, after flooding by above-mentioned definite dip time, beginning is carried out percolation with the speed of 2～3ml/min; Carried out primary sample in per 2 hours; Sample spot on same lamellae, when no sinomenine principal spot, is stopped percolation.Confirm as the terminal time of percolation.
3.3pH the value scope is investigated
After above-mentioned 3.2 percolates that obtain are regulated that pH value to 11 is above and are filtered with lime water; Obtain 5 parts of 50ml percolates; Every part extracts respectively with the 16ml chloroform after transferring to different pH value with hydrochloric acid is counter, gets extract, puts on same lamellae; Minimum with impure speckle, the maximum pH value point of principal spot is the best
The pH value range of accommodation.
3.4 extractant consumption and number of times are investigated
Get above-mentioned 3.3 percolates after filtering, the optimal pH of transferring pH to 3.3 to confirm adopts chloroform to extract; Press 1/2 percolate volume first, the consumption of each 1/3 percolation liquid extracts later on, gets extract after each extraction; Sample spot is on same lamellae; When no sinomenine speckle, end extraction, confirm that this consumption and number of times are this technological parameter.
3.5 finger printing is investigated
Extract Caulis Sinomenii coarse powder 200g by above-mentioned 3.1,3.2,3.3,3.4 definite good parameters; Respectively at percolation, alkalization filter, sour water is instead transferred, extraction, acidify crystallize, operation stage such as refining are got percolate, aqueous alkali, weak lye, extract, bullion, mother solution, elaboration; Sample spot is analyzed on same lamellae.
3.6 thin layer chromatography point plate: get the sample 5ul of above-mentioned test respectively with 5ul point sample capillary tube, put on silica gel g thin-layer plate in order.
4, result
4.1 confirming of the selection of concentration of hydrochloric acid and dip time seen table one and accompanying drawing 1 to accompanying drawing 5.
Table one: the solvent extraction of variable concentrations is in the thin layer situation of different time
Brief summary: the hydrochloric acid with above 4 groups of concentration floods, and can obtain 8-9 material (observing after ultraviolet light and the bismuth potassium iodide colour developing).And the hydrochloric acid extraction that adopts 0.1mol/L to obvious low than other three groups of concentration of main constituent, all be rational so choose the above concentration of 0.3mol/L (containing 0.3mol/L).0.3mol/L tentatively confirming as 12 hours, the dip time of hydrochloric acid reaches Cmax; 0.7mol/L tentatively confirming as 10 hours, the dip time of hydrochloric acid reaches maximum concentration; 1.0mol/L tentatively confirming as 8 hours, the dip time of hydrochloric acid reaches maximum concentration.
4.2 confirming of percolation time seen table two and accompanying drawing 6.
Table two: the thin layer situation of different time sections during percolation
Brief summary: 6 hours is that percolation is complete.Confirm to end percolation in 6-8 hour.
4.3pH confirming of value scope seen table three and accompanying drawing 7.
Table three: different PH chromatogram situation
Brief summary: confirming the 3rd point, is best pH during pH=8 promptly, is that pH=7-9 regulates allowed band between the 2nd and 4.
4.4 confirming of extractant consumption and number of times seen table four and accompanying drawing 8.
Table four: the thin layer situation of different extraction times
Brief summary: accompanying drawing 8 is followed successively by the sample that extracts 1,2,3,4 times from left to right, and under the ultraviolet, speck point is strengthened successively, and the non-main constituent amount of extraction increases.Though because of all also containing micro-main constituent in the extract of third and fourth time, by-product volume increases, and can consider to extract 2 times, the method for each 1/2 consumption extracts.
5, table five and accompanying drawing 9 are seen in the research of finger printing.
Table five: different process stage chromatogram situation
Annotate: this extract is the sample that extracts first.
Brief summary: this adopts the hydrochloric acid percolation; Can extract hydrochloric sinomenine at interior totally 9 kinds of material compositions; 7 kinds of materials are wherein arranged under ultraviolet, and the bismuth potassium iodide following 2 kinds of materials that develop the color filter weak baseization, extraction through alkalization again; Effectively a kind of non-main constituent alkaloid under observed 6 kinds of materials and the colour developing under the removal ultraviolet obtains single sinomenine hydrochloride through making with extra care again.Proof this method is scientific and reasonable, simple and feasible.
Experimental example two: contrast experiment
Chloroform reflux, extract, technology in the table six: attach the sinomenine hydrochloride standard for one one 622 pages by Chinese Pharmacopoeia version in 2010.
Benzene reflux, extract, technology in the table six: raw material pulverizing, oven dry add the alkalization of Calx mix homogeneously; Insert and add in the extraction pot that the close reflux, extract, of the full envelope of benzene concentrates, filters, cooling, separate; Obtain free sinomenine; In free sinomenine, add HCl and transform generation sinomenine hydrochloride solution, carry out recrystallization with water again and obtain the product sinomenine hydrochloride.
The result sees table six.
Table six: contrast and experiment
Following embodiment all can realize the effect of above-mentioned experimental example.
Embodiment one:
The 200g Caulis Sinomenii is dried, was pulverized 20 orders, adds 0.3mol/L HCl 160ml and in beaker, stirs, and moistening was put in the percolator after 6 hours; Add the hydrochloric acid of 0.3mol/L, make it cover liquid level 10cm, flood after 24 hours, beginning is carried out percolation with the speed of 2～3ml/min; Collect percolate after 24 hours, add lime cream and regulate pH value to 11.3, filter; Filtrating reuse HCl regulates pH value to 8.8, with chloroform extraction 4 times, lower floor's chloroform solution through dewater, concentrating under reduced pressure; Reclaim solvent, concentrated solution is regulated pH value to 2 with the hydrochloric acid of 6mol/L, and stirring, cold filtration get the sinomenine hydrochloride bullion;
Get sinomenine hydrochloride bullion 5.8g, be heated to backflow, add the 0.24g active carbon after the stirring and dissolving with 95% ethanol 90ml; Insulation refluxed 30 minutes, filtered while hot, and filtrating is concentrated into 1/5; Cooling, crystallize filter, and it is colourless to filtrating to clean filter cake with ethanol; Sinomenine hydrochloride elaboration 2.22g, relative medical material yield more than 1.11%, content 97.9%.
Sodium polyacrylate NP-700 is a framework material, and polyvinylpyrrolidone K30 is a tackifier, and glycerol is wetting agent, and Kaolin is filler, and glycosides hydroxyl aluminum is cross-linking agent, and tartaric acid is cross-linking regulator.Take by weighing sodium polyacrylate (NP-700) 2g, polyvinylpyrrolidone (K-30) 0.2g, Kaolin 5g, glycosides hydroxyl aluminum 0.3g, sinomenine hydrochloride 0.3g, mix homogeneously joins in the 25g glycerol, stirs to obtain the A phase.Transdermal enhancer Oleum menthae 0.5g and 2g sinomenine hydrochloride are added in an amount of distilled water, obtain the B phase.Transdermal enhancer comprises limonene, carvone, terpinolene etc.Take by weighing tartaric acid 0.3g, abundant dissolving obtains the C phase in the adding distilled water.With A mutually with B mix homogeneously mutually, to wherein slowly stirring adding C phase, stirred 10～20 minutes, obtain the thickness mastic.Mastic is evenly coated on the medical adhesive-bonded fabric, covered adherent layer, cut into the certain specification size, more than 24 hours, make mastic full cross-linked in 27 ℃, 50% damp condition held.
Embodiment two:
The 400g Caulis Sinomenii is dried, was pulverized 20 orders, adds 1.0mol/L HCl 300ml and in beaker, stirs, and moistening was put in the percolator after 0.5 hour; Add the hydrochloric acid of 1N, make it cover liquid level 5cm, dipping, beginning is carried out percolation with the speed of 5ml/min after 48 hours; Collect percolate after 8 hours, add lime cream and regulate pH value to 10.8, filter, filtrating reuse HCl regulates pH value to 9.2; With chloroform extraction 3 times, lower floor's chloroform solution reclaims solvent through dehydration, concentrating under reduced pressure; Concentrated solution is regulated pH value to 3.5 with the hydrochloric acid of 6mol/L, the hydrochlorate that stir, cold filtration gets sinomenine, and recrystallization gets the sinomenine hydrochloride bullion in ethanol;
Get sinomenine hydrochloride bullion 11.2g, be heated to backflow, add the 0.5g active carbon after the stirring and dissolving with 95% ethanol 110ml; Insulation refluxed 30 minutes, filtered while hot, and filtrating is concentrated into 1/4; Cooling, crystallize filter, and it is colourless to filtrating to clean filter cake with ethanol; Get sinomenine hydrochloride elaboration 4.61g, relative medical material yield 1.15%, content 96.4%.
Sodium polyacrylate NP-700 is a framework material, and polyvinylpyrrolidone K30 is a tackifier, and glycerol is wetting agent, and Kaolin is filler, and glycosides hydroxyl aluminum is cross-linking agent, and tartaric acid is cross-linking regulator.Take by weighing sodium polyacrylate (NP-700) 2g, polyvinylpyrrolidone (K-30) 0.2g, Kaolin 5g, glycosides hydroxyl aluminum 0.3g, sinomenine hydrochloride 0.3g, mix homogeneously joins in the 25g glycerol, stirs to obtain the A phase.Transdermal enhancer Oleum menthae 0.5g and 2g sinomenine hydrochloride are added in an amount of distilled water, obtain the B phase.Transdermal enhancer comprises limonene, carvone, terpinolene etc.Take by weighing tartaric acid 0.3g, abundant dissolving obtains the C phase in the adding distilled water.With A mutually with B mix homogeneously mutually, to wherein slowly stirring adding C phase, stirred 10～20 minutes, obtain the thickness mastic.Mastic is evenly coated on the medical adhesive-bonded fabric, covered adherent layer, cut into the certain specification size, more than 24 hours, make mastic full cross-linked in 27 ℃, 50% damp condition held.
Embodiment three:
The 300g Caulis Sinomenii is dried, was pulverized 10 orders, adds 0.1mol/L HCl 240ml and in beaker, stirs, and moistening was put in the percolator after 2 hours; Add the hydrochloric acid of 0.1mol/L, make it cover liquid level 8cm, flood after 36 hours, beginning is carried out percolation with the speed of 3ml/min; Collect percolate after 12 hours, add lime cream and regulate pH value to 11.5, filter, filtrating reuse HCl regulates pH value to 9.5; With chloroform extraction 5 times, lower floor's chloroform solution washing through concentrating under reduced pressure, is reclaimed solvent to neutral; Concentrated solution is regulated pH value to 2 with the hydrochloric acid of 6mol/L, the hydrochlorate that stir, cold filtration gets sinomenine, and recrystallization gets the sinomenine hydrochloride bullion in ethanol;
Get sinomenine hydrochloride bullion 7.5g, be heated to backflow, add the 0.3g active carbon after the stirring and dissolving with 95% ethanol 60ml; Insulation refluxed 30 minutes, filtered while hot, and filtrating is concentrated into 1/3; Cooling, crystallize filter, and it is colourless to filtrating to clean filter cake with ethanol; Get sinomenine hydrochloride elaboration 3.3g, relative medical material yield 1.1%, content 96.5%.
Sodium polyacrylate NP-700 is a framework material, and polyvinylpyrrolidone K30 is a tackifier, and glycerol is wetting agent, and Kaolin is filler, and glycosides hydroxyl aluminum is cross-linking agent, and tartaric acid is cross-linking regulator.Take by weighing sodium polyacrylate (NP-700) 2g, polyvinylpyrrolidone (K-30) 0.2g, Kaolin 5g, glycosides hydroxyl aluminum 0.3g, sinomenine hydrochloride 0.3g, mix homogeneously joins in the 25g glycerol, stirs to obtain the A phase.Transdermal enhancer Oleum menthae 0.5g and 2g sinomenine hydrochloride are added in an amount of distilled water, obtain the B phase.Transdermal enhancer comprises limonene, carvone, terpinolene etc.Take by weighing tartaric acid 0.3g, abundant dissolving obtains the C phase in the adding distilled water.With A mutually with B mix homogeneously mutually, to wherein slowly stirring adding C phase, stirred 10～20 minutes, obtain the thickness mastic.Mastic is evenly coated on the medical adhesive-bonded fabric, covered adherent layer, cut into the certain specification size, more than 24 hours, make mastic full cross-linked in 27 ℃, 50% damp condition held.
Embodiment four:
The 1000g Caulis Sinomenii is dried, was pulverized 20 orders, adds 0.3mol/LHCl 800ml and in beaker, stirs, and moistening was put in the percolator after 5 hours; Add the hydrochloric acid of 0.3mol/L, make it cover liquid level 2cm, flood after 6 hours, beginning is carried out percolation with the speed of 2～3ml/min; Collect percolate after 24 hours, add lime cream and regulate pH value to 11.3, filter; Filtrating reuse HCl regulates pH value to 8.8, with chloroform extraction 3 times, lower floor's chloroform solution through dewater, concentrating under reduced pressure; Reclaim solvent, concentrated solution is regulated pH value to 2 with the hydrochloric acid of 6mol/L, and stirring, cold filtration get the sinomenine hydrochloride bullion;
Get sinomenine hydrochloride bullion 4g, to dissolving fully, add the 0.16g active carbon with 75% ethanol 40ml reflux, insulation refluxed 20 minutes; Filter while hot, filtrating concentrates, cooling, crystallize; Filter, it is colourless to filtrating to clean filter cake with ethanol, gets sinomenine hydrochloride elaboration 1.62g.
Sodium polyacrylate NP-700 is a framework material, and polyvinylpyrrolidone K30 is a tackifier, and glycerol is wetting agent, and Kaolin is filler, and glycosides hydroxyl aluminum is cross-linking agent, and tartaric acid is cross-linking regulator.Take by weighing sodium polyacrylate (NP-700) 2g, polyvinylpyrrolidone (K-30) 0.2g, Kaolin 5g, glycosides hydroxyl aluminum 0.3g, sinomenine hydrochloride 0.3g, mix homogeneously joins in the 25g glycerol, stirs to obtain the A phase.Transdermal enhancer Oleum menthae 0.5g and 2g sinomenine hydrochloride are added in an amount of distilled water, obtain the B phase.Transdermal enhancer comprises limonene, carvone, terpinolene etc.Take by weighing tartaric acid 0.3g, abundant dissolving obtains the C phase in the adding distilled water.With A mutually with B mix homogeneously mutually, to wherein slowly stirring adding C phase, stirred 10～20 minutes, obtain the thickness mastic.Mastic is evenly coated on the medical adhesive-bonded fabric, covered adherent layer, cut into the certain specification size, more than 24 hours, make mastic full cross-linked in 27 ℃, 50% damp condition held.
Embodiment five:
The 1000g Caulis Sinomenii is dried, was pulverized 20 orders, adds 0.3mol/L HCl 900ml and in beaker, stirs, and moistening was put in the percolator after 8 hours; Add the hydrochloric acid of 0.3mol/L, make it cover liquid level 3cm, flood after 12 hours, beginning is carried out percolation with the speed of 2～3ml/min; Collect percolate after 6 hours, add lime cream and regulate pH value to 11.4, filter; Filtrating reuse HCl regulates pH value to 8.8, with chloroform extraction 2 times, lower floor's chloroform solution through dewater, concentrating under reduced pressure; Reclaim solvent, concentrated solution is regulated pH value to 2 with the hydrochloric acid of 6mol/L, and stirring, cold filtration get the sinomenine hydrochloride bullion;
Get sinomenine hydrochloride bullion 5g, to dissolving fully, add the 0.2g active carbon with 50% ethanol 37ml reflux, insulation refluxed 10 minutes; Filter while hot, filtrating concentrates, cooling, crystallize; Filter, it is colourless to filtrating to clean filter cake with ethanol, gets sinomenine hydrochloride elaboration 1.71g.
Sodium polyacrylate NP-700 is a framework material, and polyvinylpyrrolidone K30 is a tackifier, and glycerol is wetting agent, and Kaolin is filler, and glycosides hydroxyl aluminum is cross-linking agent, and tartaric acid is cross-linking regulator.Take by weighing sodium polyacrylate (NP-700) 2g, polyvinylpyrrolidone (K-30) 0.2g, Kaolin 5g, glycosides hydroxyl aluminum 0.3g, sinomenine hydrochloride 0.3g, mix homogeneously joins in the 25g glycerol, stirs to obtain the A phase.Transdermal enhancer Oleum menthae 0.5g and 2g sinomenine hydrochloride are added in an amount of distilled water, obtain the B phase.Transdermal enhancer comprises limonene, carvone, terpinolene etc.Take by weighing tartaric acid 0.3g, abundant dissolving obtains the C phase in the adding distilled water.With A mutually with B mix homogeneously mutually, to wherein slowly stirring adding C phase, stirred 10～20 minutes, obtain the thickness mastic.Mastic is evenly coated on the medical adhesive-bonded fabric, covered adherent layer, cut into the certain specification size, more than 24 hours, make mastic full cross-linked in 27 ℃, 50% damp condition held.
Embodiment six:
The 1000g Caulis Sinomenii is dried, was pulverized 20 orders, adds 0.3mol/L HCl 700ml and in beaker, stirs, and moistening was put in the percolator after 3 hours; Add the hydrochloric acid of 0.3mol/L, make it cover liquid level 5cm, flood after 16 hours, beginning is carried out percolation with the speed of 2～3ml/min; Collect percolate after 10 hours, add lime cream and regulate pH value to 11.1, filter; Filtrating reuse HCl regulates pH value to 8.8, with chloroform extraction 3 times, lower floor's chloroform solution through dewater, concentrating under reduced pressure; Reclaim solvent, concentrated solution is regulated pH value to 2 with the hydrochloric acid of 6mol/L, and stirring, cold filtration get the sinomenine hydrochloride bullion;
Get sinomenine hydrochloride bullion 6g, to dissolving fully, add the 0.16g active carbon with 10% ethanol 30ml reflux, insulation refluxed 16 minutes; Filter while hot, filtrating concentrates, cooling, crystallize; Filter, it is colourless to filtrating to clean filter cake with ethanol, gets sinomenine hydrochloride elaboration 1.87g.
Sodium polyacrylate NP-700 is a framework material, and polyvinylpyrrolidone K30 is a tackifier, and glycerol is wetting agent, and Kaolin is filler, and glycosides hydroxyl aluminum is cross-linking agent, and tartaric acid is cross-linking regulator.Take by weighing sodium polyacrylate (NP-700) 2g, polyvinylpyrrolidone (K-30) 0.2g, Kaolin 5g, glycosides hydroxyl aluminum 0.3g, sinomenine hydrochloride 0.3g, mix homogeneously joins in the 25g glycerol, stirs to obtain the A phase.Transdermal enhancer Oleum menthae 0.5g and 2g sinomenine hydrochloride are added in an amount of distilled water, obtain the B phase.Transdermal enhancer comprises limonene, carvone, terpinolene etc.Take by weighing tartaric acid 0.3g, abundant dissolving obtains the C phase in the adding distilled water.With A mutually with B mix homogeneously mutually, to wherein slowly stirring adding C phase, stirred 10～20 minutes, obtain the thickness mastic.Mastic is evenly coated on the medical adhesive-bonded fabric, covered adherent layer, cut into the certain specification size, more than 24 hours, make mastic full cross-linked in 27 ℃, 50% damp condition held.
Embodiment seven:
The 1000g Caulis Sinomenii is dried, was pulverized 20 orders, adds 0.3mol/L HCl 700ml and in beaker, stirs, and moistening was put in the percolator after 1 hour; Add the hydrochloric acid of 0.3mol/L, make it cover liquid level 10cm, flood after 12 hours, beginning is carried out percolation with the speed of 2～3ml/min; Collect percolate after 10 hours, add lime cream and regulate pH value to 11.3, filter; Filtrating reuse HCl regulates pH value to 8.8, with chloroform extraction 4 times, lower floor's chloroform solution through dewater, concentrating under reduced pressure; Reclaim solvent, concentrated solution is regulated pH value to 2 with the hydrochloric acid of 6mol/L, and stirring, cold filtration get the sinomenine hydrochloride bullion;
Get sinomenine hydrochloride bullion 7.8g, be heated to 80 ℃ of insulations with the 30ml purified water, the dissolving back adds the active carbon of 0.32g fully, is incubated 30 minutes; Filter while hot, filtrating concentrates, cooling, crystallize; Filter, it is colourless to filtrating to clean filter cake with ethanol, gets sinomenine hydrochloride elaboration 2.55g.
Above embodiment all no longer contains sinomenine in the raw material slag after with the hydrochloric acid percolation.The yield of sinomenine is more than 1.1% of material quantity, content 94～99%.
Sodium polyacrylate NP-700 is a framework material, and polyvinylpyrrolidone K30 is a tackifier, and glycerol is wetting agent, and Kaolin is filler, and glycosides hydroxyl aluminum is cross-linking agent, and tartaric acid is cross-linking regulator.Take by weighing sodium polyacrylate (NP-700) 2g, polyvinylpyrrolidone (K-30) 0.2g, Kaolin 5g, glycosides hydroxyl aluminum 0.3g, sinomenine hydrochloride 0.3g, mix homogeneously joins in the 25g glycerol, stirs to obtain the A phase.Transdermal enhancer Oleum menthae 0.5g and 2g sinomenine hydrochloride are added in an amount of distilled water, obtain the B phase.Transdermal enhancer comprises limonene, carvone, terpinolene etc.Take by weighing tartaric acid 0.3g, abundant dissolving obtains the C phase in the adding distilled water.With A mutually with B mix homogeneously mutually, to wherein slowly stirring adding C phase, stirred 10～20 minutes, obtain the thickness mastic.Mastic is evenly coated on the medical adhesive-bonded fabric, covered adherent layer, cut into the certain specification size, more than 24 hours, make mastic full cross-linked in 27 ℃, 50% damp condition held.
Claims (8)
1. the method for preparing of sinomenine hydrochloride cataplasma is characterized in that this method comprises the steps:
The preparation of step 1, sinomenine hydrochloride:
A, preparation sinomenine hydrochloride bullion
Extract: Caulis Sinomenii coarse powder 100～1000 weight portions, with 0.1～1mol/L HCl moistening of 60～1000 parts by volume 0.5～8 hour, adorn percolator; Adding 0.1～1mol/L HCl again makes liquid level cover medicated powder 2cm; Flood after 6～48 hours, begin percolation, stop percolation after 6～24 hours by the speed of 2～6ml/min; Get percolate, subsequent use;
Extraction: above-mentioned percolate is added lime cream transfer pH to 10.5～12.0, filter, filtrating adds hydrochloric acid and transfers pH to 7.0～9.5, with chloroform extraction 2～5 times; Combined chloroform layer water is washed till neutrality, adds the anhydrous Na2SO4 dehydration of 3%～6% times of weight, and concentrating under reduced pressure reclaims chloroform;
Crystallization: concentrated solution splashes into 6mol/L HCl and transfers pH to 2～4, and be stirred to the come-up solids and disperse, cold preservation, sucking filtration discards filtrating, and 60 ℃～70 ℃ oven dry filter cakes get yellow sinomenine hydrochloride bullion;
B, sinomenine hydrochloride process for refining
Get sinomenine hydrochloride bullion 5～10 weight portions,, add the active carbon of 4% times of weight with 10～95% ethanol or the dissolving extremely fully of purified water reflux of 30～120 parts by volume; Insulation refluxed 10～30 minutes, filtered while hot, and filtrating concentrates; Cooling, crystallize; Filter, it is colourless to filtrating that the ethanol with 95% cleans filter cake, gets sinomenine hydrochloride;
Step 2, get raw material:
Step 3, cataplasma preparation:
Take by weighing sodium polyacrylate (NP-700), polyvinylpyrrolidone (K-30), Kaolin, glycosides hydroxyl aluminum, sinomenine hydrochloride, mix homogeneously joins in the glycerol, stirs to obtain the A phase; Oleum menthae and sinomenine hydrochloride are added in the distilled water, obtain the B phase; Take by weighing tartaric acid, obtain the C phase with dissolving in the distilled water.
With A mutually with B mix homogeneously mutually, to wherein slowly stirring adding C phase, stirred 10～20 minutes, obtain the thickness mastic; Mastic is evenly coated on the medical adhesive-bonded fabric, covered adherent layer, more than 18-36 hour, make mastic full cross-linked in 25-28 ℃, 40--60% damp condition held.
2. the method for preparing of sinomenine hydrochloride cataplasma as claimed in claim 1 is characterized in that the step 1 in this method is:
A, preparation sinomenine hydrochloride bullion
Extract: Caulis Sinomenii coarse powder 500 weight portions, with the 0.5mol/L HCl moistening of 500 parts by volume 2 hours, adorn percolator; Add 0.5mol/L HCl again and make liquid level cover medicated powder 3cm, flood after 24 hours, begin percolation by the speed of 3ml/min; Stop percolation after 15 hours, get percolate, subsequent use;
Extraction: above-mentioned percolate is added lime cream transfer pH to 11.6, filter, filtrating adds hydrochloric acid and transfers pH to 8, with chloroform extraction 4 times; Combined chloroform layer water is washed till neutrality, adds the anhydrous Na2SO4 dehydration of 3% times of weight, and concentrating under reduced pressure reclaims chloroform;
Crystallization: concentrated solution splashes into 6mol/L HCl and transfers pH to 3, and be stirred to the come-up solids and disperse, cold preservation, sucking filtration discards filtrating, and 65 ℃ of oven dry filter cakes get yellow sinomenine hydrochloride bullion;
B, sinomenine hydrochloride process for refining
Get sinomenine hydrochloride bullion 7 weight portions, the concentration of using 60 parts by volume is 75% alcohol heating reflux dissolving extremely fully, adds the active carbon of 4% times of weight; Insulation refluxed 20 minutes, filtered while hot, and filtrating concentrates; Cooling, crystallize; Filter, it is colourless to filtrating that the ethanol with 95% cleans filter cake, gets sinomenine hydrochloride.
3. the method for preparing of sinomenine hydrochloride cataplasma as claimed in claim 1 is characterized in that the step 1 in this method is:
A, preparation sinomenine hydrochloride bullion
Extract: Caulis Sinomenii coarse powder 400 weight portions, with the 0.3mol/L HCl moistening of 320 parts by volume 3.5 hours, adorn percolator; Add 0.3mol/L HCl again and make liquid level cover medicated powder 4cm, flood after 6 hours, begin percolation by the speed of 6ml/min; Stop percolation after 8 hours, get percolate, subsequent use;
Extraction: above-mentioned percolate is added lime cream transfer pH to 11.3, filter, filtrating adds hydrochloric acid and transfers pH to 8.5, with chloroform extraction 2 times; Combined chloroform layer water is washed till neutrality, adds the anhydrous Na2SO4 dehydration of 5% times of weight, and concentrating under reduced pressure reclaims chloroform;
Crystallization: concentrated solution splashes into 6mol/L HCl and transfers pH to 4, and be stirred to the come-up solids and disperse, cold preservation, sucking filtration discards filtrating, and 62 ℃ of oven dry filter cakes get yellow sinomenine hydrochloride bullion;
B, sinomenine hydrochloride process for refining
Get sinomenine hydrochloride bullion 10 weight portions,, add the active carbon of 4% times of weight with the 95% alcohol heating reflux dissolving extremely fully of 120 parts by volume; Insulation refluxed 25 minutes, filtered while hot, and filtrating concentrates; Cooling, crystallize; Filter, it is colourless to filtrating that the ethanol with 95% cleans filter cake, gets sinomenine hydrochloride.
4. the method for preparing of sinomenine hydrochloride cataplasma as claimed in claim 1 is characterized in that the step 1 in this method is:
A, preparation sinomenine hydrochloride bullion
Extract: Caulis Sinomenii coarse powder 200 weight portions, with the 0.2mol/L HCl moistening of 900 parts by volume 3.5 hours, adorn percolator; Add 0.8mol/L HCl again and make liquid level cover medicated powder 4cm, flood after 15 hours, begin percolation by the speed of 4ml/min; Stop percolation after 20 hours, get percolate, subsequent use;
Extraction: above-mentioned percolate is added lime cream transfer pH to 11.3, filter, filtrating adds hydrochloric acid and transfers pH to 9, with chloroform extraction 2 times; Combined chloroform layer water is washed till neutrality, adds the anhydrous Na2SO4 dehydration of 5% times of weight, and concentrating under reduced pressure reclaims chloroform;
Crystallization: concentrated solution splashes into 6mol/L HCl and transfers pH to 4, and be stirred to the come-up solids and disperse, cold preservation, sucking filtration discards filtrating, and 62 ℃ of oven dry filter cakes get yellow sinomenine hydrochloride bullion;
B, sinomenine hydrochloride process for refining
Get sinomenine hydrochloride bullion 8 weight portions,, add the active carbon of 4% times of weight with 50% ethanol or the dissolving extremely fully of purified water reflux of 12 parts by volume; Insulation refluxed 25 minutes, filtered while hot, and filtrating concentrates; Cooling, crystallize; Filter, it is colourless to filtrating that the ethanol with 95% cleans filter cake, gets sinomenine hydrochloride.
5. the method for preparing of sinomenine hydrochloride cataplasma as claimed in claim 1 is characterized in that the step 1 in this method is:
A, preparation sinomenine hydrochloride bullion
Extract: Caulis Sinomenii coarse powder 800 weight portions, with the 0.8mol/L HCl moistening of 300 parts by volume 1 hour, adorn percolator; Add 0.2mol/L HCl again and make liquid level cover medicated powder 5cm, flood after 36 hours, begin percolation by the speed of 5ml/min; Stop percolation after 8 hours, get percolate, subsequent use;
Extraction: above-mentioned percolate is added lime cream transfer pH to 11.3, filter, filtrating adds hydrochloric acid and transfers pH to 7, with chloroform extraction 5 times; Combined chloroform layer water is washed till neutrality, adds the anhydrous Na2SO4 dehydration of 6% times of weight, and concentrating under reduced pressure reclaims chloroform;
Crystallization: concentrated solution splashes into 6mol/L HCl and transfers pH to 2, and be stirred to the come-up solids and disperse, cold preservation, sucking filtration discards filtrating, and 68 ℃ of oven dry filter cakes get yellow sinomenine hydrochloride bullion;
B, sinomenine hydrochloride process for refining
Get sinomenine hydrochloride bullion 6 weight portions,, add the active carbon of 4% times of weight with 80% ethanol or the dissolving extremely fully of purified water reflux of 40 parts by volume; Insulation refluxed 15 minutes, filtered while hot, and filtrating concentrates; Cooling, crystallize; Filter, it is colourless to filtrating that the ethanol with 95% cleans filter cake, gets sinomenine hydrochloride.
6. like the method for preparing of the arbitrary described sinomenine hydrochloride cataplasma of claim 1-5, it is characterized in that the step 2 in this method is:
7. like the method for preparing of the arbitrary described sinomenine hydrochloride cataplasma of claim 1-5, it is characterized in that the step 3 in this method is:
Take by weighing sodium polyacrylate, polyvinylpyrrolidone, Kaolin,, glycosides hydroxyl aluminum, sinomenine hydrochloride, mix homogeneously joins in the glycerol, stirs to obtain the A phase; Transdermal enhancer Oleum menthae and sinomenine hydrochloride are added in the distilled water, obtain the B phase; Take by weighing tartaric acid, obtain the C phase with dissolved in distilled water; With A mutually with B mix homogeneously mutually, to wherein slowly stirring adding C phase, stirred 10～20 minutes, obtain the thickness mastic; Mastic is evenly coated on the medical adhesive-bonded fabric, covered adherent layer, cut into the certain specification size, more than 24 hours, make mastic full cross-linked in 27 ℃, 50% damp condition held.
8. the method for preparing of sinomenine hydrochloride cataplasma as claimed in claim 6 is characterized in that the step 3 in this method is:
Take by weighing sodium polyacrylate, polyvinylpyrrolidone, Kaolin,, glycosides hydroxyl aluminum, sinomenine hydrochloride, mix homogeneously joins in the glycerol, stirs to obtain the A phase; Transdermal enhancer Oleum menthae and sinomenine hydrochloride are added in the distilled water, obtain the B phase; Take by weighing tartaric acid, obtain the C phase with dissolved in distilled water; With A mutually with B mix homogeneously mutually, to wherein slowly stirring adding C phase, stirred 10～20 minutes, obtain the thickness mastic; Mastic is evenly coated on the medical adhesive-bonded fabric, covered adherent layer, cut into the certain specification size, more than 24 hours, make mastic full cross-linked in 27 ℃, 50% damp condition held.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106137949A (en) * | 2016-08-04 | 2016-11-23 | 长沙原道医药科技开发有限公司 | Sinomenine hydrochloride ointment prepared by a kind of inorganic solvent and preparation method thereof |
| CN106176686A (en) * | 2016-08-04 | 2016-12-07 | 长沙原道医药科技开发有限公司 | Sinomenine hydrochloride liniment prepared by a kind of inorganic solvent and preparation method thereof |
| CN106176578A (en) * | 2016-08-04 | 2016-12-07 | 长沙原道医药科技开发有限公司 | Sinomenine hydrochloride gel prepared by a kind of organic solvent and preparation method thereof |
| CN106176577A (en) * | 2016-08-04 | 2016-12-07 | 长沙原道医药科技开发有限公司 | Sinomenine hydrochloride gel prepared by a kind of inorganic solvent and preparation method thereof |
| CN106236700A (en) * | 2016-08-04 | 2016-12-21 | 长沙原道医药科技开发有限公司 | Sinomenine hydrochloride ointment prepared by a kind of organic solvent and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106137949A (en) * | 2016-08-04 | 2016-11-23 | 长沙原道医药科技开发有限公司 | Sinomenine hydrochloride ointment prepared by a kind of inorganic solvent and preparation method thereof |
| CN106176686A (en) * | 2016-08-04 | 2016-12-07 | 长沙原道医药科技开发有限公司 | Sinomenine hydrochloride liniment prepared by a kind of inorganic solvent and preparation method thereof |
| CN106176578A (en) * | 2016-08-04 | 2016-12-07 | 长沙原道医药科技开发有限公司 | Sinomenine hydrochloride gel prepared by a kind of organic solvent and preparation method thereof |
| CN106176577A (en) * | 2016-08-04 | 2016-12-07 | 长沙原道医药科技开发有限公司 | Sinomenine hydrochloride gel prepared by a kind of inorganic solvent and preparation method thereof |
| CN106236700A (en) * | 2016-08-04 | 2016-12-21 | 长沙原道医药科技开发有限公司 | Sinomenine hydrochloride ointment prepared by a kind of organic solvent and preparation method thereof |
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