CN103690759B - Compound liquorice-fritillarithunbergii-ammonium thunbergii-ammonium chloride medicinal composition and preparation method thereof - Google Patents
Compound liquorice-fritillarithunbergii-ammonium thunbergii-ammonium chloride medicinal composition and preparation method thereof Download PDFInfo
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- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 239000000203 mixture Substances 0.000 title claims abstract description 24
- 150000001875 compounds Chemical class 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims description 67
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 52
- 239000012530 fluid Substances 0.000 claims abstract description 46
- 239000008194 pharmaceutical composition Substances 0.000 claims abstract description 35
- 239000000843 powder Substances 0.000 claims abstract description 35
- 239000003814 drug Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000008187 granular material Substances 0.000 claims description 76
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 58
- 239000003826 tablet Substances 0.000 claims description 58
- 239000007788 liquid Substances 0.000 claims description 48
- 238000001914 filtration Methods 0.000 claims description 46
- 239000000243 solution Substances 0.000 claims description 30
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 24
- 239000000725 suspension Substances 0.000 claims description 21
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 20
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 20
- 238000005325 percolation Methods 0.000 claims description 20
- 239000002244 precipitate Substances 0.000 claims description 20
- 239000011248 coating agent Substances 0.000 claims description 19
- 238000000576 coating method Methods 0.000 claims description 19
- 239000012047 saturated solution Substances 0.000 claims description 19
- 230000001476 alcoholic effect Effects 0.000 claims description 18
- 229940079593 drug Drugs 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 16
- 229920001353 Dextrin Polymers 0.000 claims description 10
- 239000004375 Dextrin Substances 0.000 claims description 10
- 229920002472 Starch Polymers 0.000 claims description 10
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 10
- 235000010216 calcium carbonate Nutrition 0.000 claims description 10
- 235000019425 dextrin Nutrition 0.000 claims description 10
- 239000007779 soft material Substances 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 239000008107 starch Substances 0.000 claims description 10
- 235000019698 starch Nutrition 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 7
- 230000008020 evaporation Effects 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000002671 adjuvant Substances 0.000 claims description 4
- 235000006753 Platycodon grandiflorum Nutrition 0.000 claims description 3
- 240000003582 Platycodon grandiflorus Species 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 238000005352 clarification Methods 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000002481 ethanol extraction Methods 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 239000002775 capsule Substances 0.000 claims description 2
- 239000000341 volatile oil Substances 0.000 abstract description 24
- 238000005516 engineering process Methods 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 239000003094 microcapsule Substances 0.000 abstract description 9
- 238000003860 storage Methods 0.000 abstract description 5
- -1 Glycyrrhiza compound Chemical class 0.000 description 46
- 241000202807 Glycyrrhiza Species 0.000 description 39
- 239000002994 raw material Substances 0.000 description 14
- 238000012360 testing method Methods 0.000 description 14
- 239000007888 film coating Substances 0.000 description 9
- 238000009501 film coating Methods 0.000 description 9
- 230000033228 biological regulation Effects 0.000 description 7
- 239000003921 oil Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 206010006451 bronchitis Diseases 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 206010006458 Bronchitis chronic Diseases 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- VTAJIXDZFCRWBR-UHFFFAOYSA-N Licoricesaponin B2 Natural products C1C(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2)C(O)=O)C)(C)CC2)(C)C2C(C)(C)CC1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O VTAJIXDZFCRWBR-UHFFFAOYSA-N 0.000 description 1
- 206010036790 Productive cough Diseases 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 208000007451 chronic bronchitis Diseases 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007941 film coated tablet Substances 0.000 description 1
- LPLVUJXQOOQHMX-UHFFFAOYSA-N glycyrrhetinic acid glycoside Natural products C1CC(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2=O)C(O)=O)C)(C)CC2)(C)C2C(C)(C)C1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O LPLVUJXQOOQHMX-UHFFFAOYSA-N 0.000 description 1
- 239000001685 glycyrrhizic acid Substances 0.000 description 1
- 229960004949 glycyrrhizic acid Drugs 0.000 description 1
- UYRUBYNTXSDKQT-UHFFFAOYSA-N glycyrrhizic acid Natural products CC1(C)C(CCC2(C)C1CCC3(C)C2C(=O)C=C4C5CC(C)(CCC5(C)CCC34C)C(=O)O)OC6OC(C(O)C(O)C6OC7OC(O)C(O)C(O)C7C(=O)O)C(=O)O UYRUBYNTXSDKQT-UHFFFAOYSA-N 0.000 description 1
- 235000019410 glycyrrhizin Nutrition 0.000 description 1
- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
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- Medicinal Preparation (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
The invention provides a kind of compound liquorice-fritillarithunbergii-ammonium thunbergii-ammonium chloride medicinal composition, this pharmaceutical composition comprises: 0.48-1.2 parts by volume Radix Polygalae fluid extractum, 0.32-0.8 parts by volume Bulbus Fritillariae Thunbergii fluid extract, 0.48-1.2 parts by volume Radix Platycodonis fluidextract, 0.8-2 parts by volume Radix Glycyrrhizae fluidextract, 0.035-0.08 parts by volume Oleum Anisi Stellati, 0.32-0.8 weight portion Radix Glycyrrhizae extractum powder, 0.4-1 weight portion ammonium chloride and 0.42-0.88 weight portion beta-schardinger dextrin-, wherein, described Oleum Anisi Stellati and described beta-schardinger dextrin-form clathrate, and described parts by volume and weight ratio are ml/g or L/kg.Compound liquorice-fritillarithunbergii-ammonium thunbergii-ammonium chloride medicinal composition of the present invention adopts microcapsule technology that ethereal oil is made microcapsule, ethereal oil can be reduced producing and the volatilization in storage process, strengthen the stability of ethereal oil, thus improve the stability of medicine, and can suitability for industrialized production be realized.
Description
Technical field
The invention belongs to pharmaceutical field, relate to a kind of pharmaceutical composition and preparation method thereof, be specifically related to a kind of compound liquorice-fritillarithunbergii-ammonium thunbergii-ammonium chloride medicinal composition and preparation method thereof.
Background technology
Glycyrrhiza compound Bulbus Fritillariae Thunbergii voltoide has been widely used for many years, is mainly used in treating cough, expectoration etc. that acute and chronic bronchitis causes, from the report of listing so far there are no untoward reaction.At present, glycyrrhiza compound Bulbus Fritillariae Thunbergii voltoide on market mainly adopts traditional tablet manufacturing technique to make, in the process, the method that effective ingredient (volatile oil) in prescription adopts dissolve with ethanol to spray into granule is added, because volatile oil has strong volatility, cause the less stable of the glycyrrhiza compound Bulbus Fritillariae Thunbergii voltoide adopting this explained hereafter, especially in production with storage process, cannot ensure that by the impact of physical factor the long-term stability of volatile oil component exists, when medicine arrives in patient's hands, the volatile oil that plaing induces sweat acts on almost is lost and is made a gift of to the greatest extent.In addition, the production technology of the glycyrrhiza compound Bulbus Fritillariae Thunbergii voltoide adopted at present focuses mostly in laboratory research, not yet realizes suitability for industrialized production.
Therefore, how to develop a kind of production technology realizing the glycyrrhiza compound Bulbus Fritillariae Thunbergii voltoide of suitability for industrialized production, reduce volatile ingredient in glycyrrhiza compound Bulbus Fritillariae Thunbergii voltoide, producing and the volatilization in storage process, to improve the stability of medicine, become the problem that this area is urgently to be resolved hurrily.
Summary of the invention
For the problems referred to above, one object of the present invention is to provide a kind of compound liquorice-fritillarithunbergii-ammonium thunbergii-ammonium chloride medicinal composition, this compound liquorice-fritillarithunbergii-ammonium thunbergii-ammonium chloride medicinal composition adopts microcapsule technology that ethereal oil is made microcapsule, ethereal oil can be reduced producing and the volatilization in storage process, strengthen the stability of ethereal oil, thus improve the stability of medicine, and suitability for industrialized production can be realized.
Another object of the present invention is to the preparation method that a kind of compound liquorice-fritillarithunbergii-ammonium thunbergii-ammonium chloride medicinal composition is provided.
For achieving the above object, the invention provides a kind of compound liquorice-fritillarithunbergii-ammonium thunbergii-ammonium chloride medicinal composition, this pharmaceutical composition comprises:
Wherein, described Oleum Anisi Stellati and described beta-schardinger dextrin-form clathrate, and described parts by volume and weight ratio are ml/g or L/kg.
Further, described pharmaceutical composition comprises:
Preferably, described pharmaceutical composition comprises:
Further, described pharmaceutical composition is tablet, capsule or granule; Preferably, described pharmaceutical composition also comprises pharmaceutically acceptable adjuvant.
Further, described pharmaceutical composition is tablet; Preferably, described pharmaceutical composition also comprises:
Starch 1.36-7.9 weight portion film coating powder 0.2-0.48 weight portion
Dextrin 0.24-1.05 weight parts of calcium carbonate 0.48-1.2 weight portion.
Further, the preparation method of described Radix Polygalae fluid extractum comprises the following steps:
Radix Polygalae powder is broken into 65 orders, use 60%(volume ratio) ethanol water make solvent, flood after 24 hours, the speed of dividing with 1-3ml/ carries out percolation, collect the first liquid of filtering of 85%, another extracting container preserves liquid of just filtering, continue percolation, after soluble component is filtered out completely, collection is filtered liquid, and below 60 DEG C cryoconcentration to paste, add the initial first liquid of filtering preserved, mixing, drip concentrated ammonia solution and make the micro-aobvious alkalescence of filtrate, and have ammonia smelly, preferred dropping 25-28%(volume ratio) concentrated ammonia solution make the pH value of filtrate be 9-10, then use 60%(volume ratio) ethanol water be diluted to crude drug weight, making ethanol content is 38-48%(volume ratio) fluid extract, leave standstill, filter after clarification and obtain described Radix Polygalae fluid extractum.
Further, the preparation method of described Bulbus Fritillariae Thunbergii fluid extract comprises the following steps:
Bulbus Fritillariae Thunbergii is ground into 24 orders, use 70%(volume ratio) ethanol water make solvent, flood after 18 hours, the speed of dividing with 1-3ml/ carries out percolation, collect the first liquid of filtering of 85%, another extracting container preserves liquid of just filtering, continue percolation, after soluble component is filtered out completely, by remaining filter liquid below 60 DEG C low-temperature evaporation to paste, add the initial first liquid of filtering preserved, mixing, add 70%(volume ratio again) ethanol water be diluted to crude drug weight, making ethanol content is 50-70%(volume ratio) fluid extract, mixing, leave standstill, described Bulbus Fritillariae Thunbergii fluid extract is obtained after filtration.
Further, the preparation method of described Radix Platycodonis fluidextract comprises the following steps:
Balloonflower powder is broken into 24 orders, use 55%(volume ratio) ethanol water make solvent, flood after 48 hours, the slow percolation of the speed of dividing with 1-3ml/, collect the first liquid of filtering of 85%, another extracting container preserves liquid of just filtering, continue percolation, after soluble component is filtered out completely, by remaining filter liquid below 60 DEG C low-temperature evaporation to paste, add the initial first liquid of filtering preserved, mixing, add 55%(volume ratio again) ethanol water be diluted to crude drug weight, making ethanol content is 40-50%(volume ratio) fluid extract, mixing, leave standstill, described Radix Platycodonis fluidextract is obtained after filtration.
Further, the preparation method of described Radix Glycyrrhizae extractum powder comprises the following steps:
By Radix Glycyrrhizae extracting in water three times, each 2 hours, merge extractive liquid, placed extracting solution and spends the night, extracting solution is precipitated, then gets supernatant concentration to paste, crushed after being dried to 80 order, obtain described Radix Glycyrrhizae extractum powder.
Further, the preparation method of described Radix Glycyrrhizae fluidextract comprises the following steps:
(1) by Radix Glycyrrhizae extracting in water three times, each 2 hours, merge extractive liquid, placed extracting solution and spends the night, extracting solution is precipitated, then gets supernatant concentration to paste, crushed after being dried to 80 order, obtain described Radix Glycyrrhizae extractum powder;
(2) by described Radix Glycyrrhizae extractum powder, use 92%(volume ratio) ethanol extraction three times, merge extractive liquid, reclaims ethanol, add suitable quantity of water and 92%(volume ratio) ethanol dilution to crude drug weight, making ethanol content is 20-25%(volume ratio) Radix Glycyrrhizae fluidextract.
Further, the method that described Oleum Anisi Stellati and beta-schardinger dextrin-form clathrate comprises the following steps:
Get Oleum Anisi Stellati to add ethanol and be mixed with 65%(volume ratio) Oleum Anisi Stellati alcoholic solution, at 56-60 DEG C, preferably at 60 DEG C by water-soluble for beta-schardinger dextrin-preparation β-CD saturated solution, at 40 DEG C, Oleum Anisi Stellati alcoholic solution is mixed with beta-schardinger dextrin-saturated solution, stir under 850 revs/min and obtain milky suspension in 2 hours, by described milky suspension at 2-6 DEG C, preferably leave standstill 24-36 hour at 4 DEG C, preferably 24 hours, white precipitate is obtained after filtration, by described white precipitate dry 3-8 hour at 45 DEG C, preferably by described white precipitate first dry 2-3h in 45 DEG C of low-temperature vacuum drying baking ovens, after most of moisture is volatilized, then in 45 DEG C of heated-air circulation ovens, 5h is placed, obtain described Oleum Anisi Stellati clathrate.
The present invention further provides the preparation method of aforementioned pharmaceutical compositions, this preparation method comprises the following steps:
Step a: Radix Polygalae fluid extractum, Bulbus Fritillariae Thunbergii fluid extract, Radix Platycodonis fluidextract, Radix Glycyrrhizae fluidextract, Radix Glycyrrhizae extractum, ammonium chloride, calcium carbonate, starch and dextrin mixed, mixes thoroughly, make granule after drying;
Step b: Oleum Anisi Stellati is mixed with the granule that step a obtains with the clathrate of beta-schardinger dextrin-.
Further, described preparation method is further comprising the steps of:
The mixture obtained to step b adds pharmaceutically acceptable adjuvant, and after soft material processed, granulation, obtain wet granular, at 60 DEG C, dry described wet granular, obtains dry granule after the granulate that sieves, and carries out tabletting, coating to described dry granule, obtained tablet.
Compared with prior art, compound liquorice-fritillarithunbergii-ammonium thunbergii-ammonium chloride medicinal composition provided by the invention and preparation method thereof has the following advantages:
One, the present invention adopts microcapsule technology (making clathrate (microcapsule) by the ethereal oil in compositions) to prepare glycyrrhiza compound Bulbus Fritillariae Thunbergii voltoide compositions, significantly improve the physicochemical property of glycyrrhiza compound Bulbus Fritillariae Thunbergii voltoide, decrease Oleum Anisi Stellati producing and the volatilization in storage process, enhance the stability of Oleum Anisi Stellati, thus improve the stability of medicine, ensure that the curative effect of medicine;
Two, the present invention adopts microcapsule technology to prepare compound liquorice-fritillarithunbergii-ammonium thunbergii-ammonium chloride medicinal composition, improves the dissolubility of insoluble drug, can cover stink and the zest of medicine (Oleum Anisi Stellati) simultaneously;
Three, the present invention adopts microcapsule technology to prepare the production technology of compound liquorice-fritillarithunbergii-ammonium thunbergii-ammonium chloride medicinal composition, and enclose mild condition, technique is simple, be easy to control, enclose productive rate is high, constant product quality, is conducive to realizing industrialization.
Detailed description of the invention
Referring to specific embodiment, the present invention is described.It will be appreciated by those skilled in the art that these embodiments are only for illustration of the present invention, its scope do not limited the present invention in any way.
Experimental technique in following embodiment, if no special instructions, is conventional method.Medicinal raw material used in following embodiment, reagent material etc., if no special instructions, be commercially available purchase product.
embodiment 1glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet 1
Prepared by raw material:
The preparation of Bulbus Fritillariae Thunbergii fluid extract: Bulbus Fritillariae Thunbergii is ground into 24 orders, use 70%(volume ratio) ethanol water make solvent, flood after 18 hours, the speed of dividing with 1-3ml/ carries out percolation, collect the first liquid of filtering of 85%, another extracting container preserves liquid of just filtering, continue percolation, after soluble component is filtered out completely, by remaining filter liquid below 60 DEG C low-temperature evaporation to paste, add the initial first liquid of filtering preserved, mixing, add 70%(volume ratio again) ethanol water be diluted to crude drug weight, making ethanol content is 50-70%(volume ratio) fluid extract, mixing, leave standstill, Bulbus Fritillariae Thunbergii fluid extract is obtained after filtration.
The preparation of Radix Platycodonis fluidextract: balloonflower powder is broken into 24 orders, use 55%(volume ratio) ethanol water make solvent, flood after 48 hours, with the slow percolation of the speed of 1-3ml/min, collect the first liquid of filtering of 85%, another extracting container preserves liquid of just filtering, continue percolation, after soluble component is filtered out completely, by remaining filter liquid below 60 DEG C low-temperature evaporation to paste, add the initial first liquid of filtering preserved, mixing, add 55%(volume ratio again) ethanol water be diluted to crude drug weight, making ethanol content is 40-50%(volume ratio) fluid extract, mixing, leave standstill, described Radix Platycodonis fluidextract is obtained after filtration,
The preparation of Radix Polygalae fluid extractum: Radix Polygalae powder is broken into 65 orders, use 60%(volume ratio) ethanol water make solvent, flood after 24 hours, slowly percolation is carried out with the speed of 1-3ml/min, collect the first liquid of filtering of 85%, another extracting container preserves liquid of just filtering, continue percolation, after soluble component is filtered out completely, collection is filtered liquid, and below 60 DEG C low-temperature evaporation to paste, add initial first filtrate of preserving, mixing, drip 25-28%(volume ratio) concentrated ammonia solution make filtrate be micro-aobvious alkalescence (pH value is 9-10), and have ammonia smelly, then use 60%(volume ratio) ethanol water be diluted to crude drug weight, making ethanol content is 38-48%(volume ratio) fluid extract, leave standstill, described Radix Polygalae fluid extractum is obtained after filtration,
The preparation of Radix Glycyrrhizae extractum fine powder: by Radix Glycyrrhizae extracting in water three times (wherein add water to and flood Radix Glycyrrhizae), each 2 hours, merge extractive liquid, extracting solution is placed and spends the night, extracting solution is precipitated, then gets supernatant concentration to paste, crushed after being dried to 80 order, obtains Radix Glycyrrhizae extractum fine powder;
The preparation of Radix Glycyrrhizae fluidextract: by Radix Glycyrrhizae extracting in water three times, each 2 hours, merge extractive liquid, extracting solution is placed and spends the night, extracting solution is precipitated, then gets supernatant concentration to paste, obtain Radix Glycyrrhizae extractum, by Radix Glycyrrhizae extractum crushed after being dried to 80 order, then use 92%(volume ratio) ethanol extraction three times, merge extractive liquid, reclaims ethanol, add suitable quantity of water and 92%(volume ratio) ethanol dilution to crude drug weight, making ethanol content is 20-25%(volume ratio) Radix Glycyrrhizae fluidextract.
The preparation of glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet:
Step a: take 0.96L Radix Polygalae fluid extractum, 0.64L Bulbus Fritillariae Thunbergii fluid extract, 0.96L Radix Platycodonis fluidextract, 1.6L Radix Glycyrrhizae fluidextract, 0.64kg Radix Glycyrrhizae extractum fine powder, 0.8kg ammonium chloride, 0.96kg calcium carbonate, 7.9kg starch and 0.83kg dextrin, and mixed, mix thoroughly, make granule after drying;
Step b: 0.07L Oleum Anisi Stellati is dissolved in ethanol, preparation 65%(volume ratio) Oleum Anisi Stellati alcoholic solution, and by 0.42kg β-CD water-soluble preparation β-CD saturated solution at 60 DEG C, then at 40 DEG C, the Oleum Anisi Stellati alcoholic solution of preparation is mixed with β-CD saturated solution, stir under 850r/min and obtain milky suspension in 2 hours, described milky suspension is left standstill 24 hours at 4 DEG C, white precipitate is obtained after filtration, by described white precipitate at 45 DEG C of low-temperature vacuum drying baking oven (ZDF-15, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing) in dry 2-3h, after most of moisture is volatilized, then at 45 DEG C of heated-air circulation oven (GT-G-II, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing) middle placement 5h, obtain Oleum Anisi Stellati clathrate,
Step c: the Oleum Anisi Stellati clathrate obtained in step b is mixed with the granule obtained in step a, through soft material processed, granulate and (adopt oscillating granulator (YK-160, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing)) after obtain wet granular, dry described wet granular at 60 DEG C, sieve after granulate and obtain dry granule, described dry granule is mixed with 0.38kg film coating powder, adopt rotary tablet machine (ZPY-23E, Shanghai Jiangnan Pharmaceutical Machinary Co., Ltd) tabletting is carried out to described dry granule, and adopt high-efficiency coating machine (BG-80, king's pharmaceutical machine Equipment Limited, sea, Nanjing) coating is carried out to described granule, obtain glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet 1.
embodiment 2glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet 2
Prepared by raw material:
With reference to the preparation method of each raw material in embodiment 1.
The preparation of glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet:
Step a: take 0.9L Radix Polygalae fluid extractum, 0.8L Bulbus Fritillariae Thunbergii fluid extract, 1.2L Radix Platycodonis fluidextract, 2L Radix Glycyrrhizae fluidextract, 0.64kg Radix Glycyrrhizae extractum fine powder, 0.8kg ammonium chloride, 1.1kg calcium carbonate, 7.9kg starch and 0.83kg dextrin, and mixed, mix thoroughly, make granule after drying;
Step b: 0.07L Oleum Anisi Stellati is dissolved in ethanol, preparation 65%(volume ratio) Oleum Anisi Stellati alcoholic solution, and by 0.56kg β-CD water-soluble preparation β-CD saturated solution at 60 DEG C, then at 40 DEG C, the Oleum Anisi Stellati alcoholic solution of preparation is mixed with β-CD saturated solution, stir under 850r/min and obtain milky suspension in 2 hours, described milky suspension is left standstill 24 hours at 4 DEG C, white precipitate is obtained after filtration, by described white precipitate at 45 DEG C of low-temperature vacuum drying baking oven (ZDF-15, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing) in dry 2-3h, after most of moisture is volatilized, then at 45 DEG C of heated-air circulation oven (GT-G-II, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing) middle placement 5h, obtain Oleum Anisi Stellati clathrate,
Step c: the Oleum Anisi Stellati clathrate obtained in step b is mixed with the granule obtained in step a, through soft material processed, granulate and (adopt oscillating granulator (YK-160, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing)) after obtain wet granular, dry described wet granular at 60 DEG C, sieve after granulate and obtain dry granule, described dry granule is mixed with 0.38kg film coating powder, adopt rotary tablet machine (ZPY-23E, Shanghai Jiangnan Pharmaceutical Machinary Co., Ltd) tabletting is carried out to described dry granule, and adopt high-efficiency coating machine (BG-80, king's pharmaceutical machine Equipment Limited, sea, Nanjing) coating is carried out to described granule, obtain glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet 2.
embodiment 3glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet 3
Prepared by raw material:
With reference to the preparation method of each raw material in embodiment 1.
The preparation of glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet:
Step a: take 0.7L Radix Polygalae fluid extractum, 0.64L Bulbus Fritillariae Thunbergii fluid extract, 0.9L Radix Platycodonis fluidextract, 0.8L Radix Glycyrrhizae fluidextract, 0.4kg Radix Glycyrrhizae extractum fine powder, 0.5kg ammonium chloride, 1.2kg calcium carbonate, 7.9kg starch and 0.83kg dextrin, and mixed, mix thoroughly, make granule after drying;
Step b: 0.04L Oleum Anisi Stellati is dissolved in ethanol, preparation 65%(volume ratio) Oleum Anisi Stellati alcoholic solution, and by 0.44kg β-CD water-soluble preparation β-CD saturated solution at 60 DEG C, then at 40 DEG C, the Oleum Anisi Stellati alcoholic solution of preparation is mixed with β-CD saturated solution, stir under 850r/min and obtain milky suspension in 2 hours, described milky suspension is left standstill 24 hours at 4 DEG C, white precipitate is obtained after filtration, by described white precipitate at 45 DEG C of low-temperature vacuum drying baking oven (ZDF-15, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing) in dry 2-3h, after most of moisture is volatilized, then at 45 DEG C of heated-air circulation oven (GT-G-II, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing) middle placement 5h, obtain Oleum Anisi Stellati clathrate,
Step c: the Oleum Anisi Stellati clathrate obtained in step b is mixed with the granule obtained in step a, through soft material processed, granulate and (adopt oscillating granulator (YK-160, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing)) after obtain wet granular, dry described wet granular at 60 DEG C, sieve after granulate and obtain dry granule, described dry granule is mixed with 0.38kg film coating powder, adopt rotary tablet machine (ZPY-23E, Shanghai Jiangnan Pharmaceutical Machinary Co., Ltd) tabletting is carried out to described dry granule, and adopt high-efficiency coating machine (BG-80, king's pharmaceutical machine Equipment Limited, sea, Nanjing) coating is carried out to described granule, obtain glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet 3.
embodiment 4glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet 4
Prepared by raw material:
With reference to the preparation method of each raw material in embodiment 1.
The preparation of glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet:
Step a: take 0.6L Radix Polygalae fluid extractum, 0.5L Bulbus Fritillariae Thunbergii fluid extract, 0.48L Radix Platycodonis fluidextract, 1.2L Radix Glycyrrhizae fluidextract, 0.8kg Radix Glycyrrhizae extractum fine powder, 0.7kg ammonium chloride, 0.84kg calcium carbonate, 6.92kg starch and 0.72kg dextrin, and mixed, mix thoroughly, make granule after drying;
Step b: 0.05L Oleum Anisi Stellati is dissolved in ethanol, preparation 65%(volume ratio) Oleum Anisi Stellati alcoholic solution, and by 0.55kg β-CD water-soluble preparation β-CD saturated solution at 60 DEG C, then at 40 DEG C, the Oleum Anisi Stellati alcoholic solution of preparation is mixed with β-CD saturated solution, stir under 850r/min and obtain milky suspension in 2 hours, described milky suspension is left standstill 24.5 hours at 4 DEG C, white precipitate is obtained after filtration, by described white precipitate at 45 DEG C of low-temperature vacuum drying baking oven (ZDF-15, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing) in dry 2-3h, after most of moisture is volatilized, then at 45 DEG C of heated-air circulation oven (GT-G-II, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing) middle placement 5h, obtain Oleum Anisi Stellati clathrate,
Step c: the Oleum Anisi Stellati clathrate obtained in step b is mixed with the granule obtained in step a, through soft material processed, granulate and (adopt oscillating granulator (YK-160, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing)) after obtain wet granular, dry described wet granular at 60 DEG C, sieve after granulate and obtain dry granule, described dry granule is mixed with 0.34kg film coating powder, adopt rotary tablet machine (ZPY-23E, Shanghai Jiangnan Pharmaceutical Machinary Co., Ltd) tabletting is carried out to described dry granule, and adopt high-efficiency coating machine (BG-80, king's pharmaceutical machine Equipment Limited, sea, Nanjing) coating is carried out to described granule, obtain glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet 4.
embodiment 5glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet 5
Prepared by raw material:
With reference to the preparation method of each raw material in embodiment 1.
The preparation of glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet:
Step a: take 0.48L Radix Polygalae fluid extractum, 0.32L Bulbus Fritillariae Thunbergii fluid extract, 0.6L Radix Platycodonis fluidextract, 1L Radix Glycyrrhizae fluidextract, 0.32kg Radix Glycyrrhizae extractum fine powder, 0.4kg ammonium chloride, 0.48kg calcium carbonate, 1.36kg starch and 0.24kg dextrin, and mixed, mix thoroughly, make granule after drying;
Step b: 0.035L Oleum Anisi Stellati is dissolved in ethanol, preparation 65%(volume ratio) Oleum Anisi Stellati alcoholic solution, and by 0.8kg β-CD water-soluble preparation β-CD saturated solution at 60 DEG C, then at 40 DEG C, the Oleum Anisi Stellati alcoholic solution of preparation is mixed with β-CD saturated solution, stir under 850r/min and obtain milky suspension in 2 hours, described milky suspension is left standstill 24.5 hours at 4 DEG C, white precipitate is obtained after filtration, by described white precipitate at 45 DEG C of low-temperature vacuum drying baking oven (ZDF-15, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing) in dry 2-3h, after most of moisture is volatilized, then at 45 DEG C of heated-air circulation oven (GT-G-II, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing) middle placement 5h, obtain Oleum Anisi Stellati clathrate,
Step c: the Oleum Anisi Stellati clathrate obtained in step b is mixed with the granule obtained in step a, through soft material processed, granulate and (adopt oscillating granulator (YK-160, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing)) after obtain wet granular, dry described wet granular at 60 DEG C, sieve after granulate and obtain dry granule, described dry granule is mixed with 0.48kg film coating powder, adopt rotary tablet machine (ZPY-23E, Shanghai Jiangnan Pharmaceutical Machinary Co., Ltd) tabletting is carried out to described dry granule, and adopt high-efficiency coating machine (BG-80, king's pharmaceutical machine Equipment Limited, sea, Nanjing) coating is carried out to described granule, obtain glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet 5.
embodiment 6glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet 6
Prepared by raw material:
With reference to the preparation method of each raw material in embodiment 1.
The preparation of glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet:
Step a: take 1.2L Radix Polygalae fluid extractum, 0.7L Bulbus Fritillariae Thunbergii fluid extract, 1L Radix Platycodonis fluidextract, 1.7L Radix Glycyrrhizae fluidextract, 0.8kg Radix Glycyrrhizae extractum fine powder, 1kg ammonium chloride, 0.6kg calcium carbonate, 7.35kg starch and 1.05kg dextrin, and mixed, mix thoroughly, make granule after drying;
Step b: 0.08L Oleum Anisi Stellati is dissolved in ethanol, preparation 65%(volume ratio) Oleum Anisi Stellati alcoholic solution, and by 0.88kg β-CD water-soluble preparation β-CD saturated solution at 60 DEG C, then at 40 DEG C, the Oleum Anisi Stellati alcoholic solution of preparation is mixed with β-CD saturated solution, stir under 850r/min and obtain milky suspension in 2 hours, described milky suspension is left standstill 24 hours at 4 DEG C, white precipitate is obtained after filtration, by described white precipitate at 45 DEG C of low-temperature vacuum drying baking oven (ZDF-15, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing) in dry 2-3h, after most of moisture is volatilized, then at 45 DEG C of heated-air circulation oven (GT-G-II, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing) middle placement 5h, obtain Oleum Anisi Stellati clathrate,
Step c: the Oleum Anisi Stellati clathrate obtained in step b is mixed with the granule obtained in step a, through soft material processed, granulate and (adopt oscillating granulator (YK-160, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing)) after obtain wet granular, dry described wet granular at 60 DEG C, sieve after granulate and obtain dry granule, described dry granule is mixed with 0.48kg film coating powder, adopt rotary tablet machine (ZPY-23E, Shanghai Jiangnan Pharmaceutical Machinary Co., Ltd) tabletting is carried out to described dry granule, and adopt high-efficiency coating machine (BG-80, king's pharmaceutical machine Equipment Limited, sea, Nanjing) coating is carried out to described granule, obtain glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet 6.
embodiment 7glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet 7
Prepared by raw material:
With reference to the preparation method of each raw material in embodiment 1.
The preparation of glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet:
Step a: take 0.8L Radix Polygalae fluid extractum, 0.6L Bulbus Fritillariae Thunbergii fluid extract, 0.96L Radix Platycodonis fluidextract, 1.5L Radix Glycyrrhizae fluidextract, 0.5kg Radix Glycyrrhizae extractum fine powder, 0.7kg ammonium chloride, 0.96kg calcium carbonate, 4.5kg starch and 0.5kg dextrin, and mixed, mix thoroughly, make granule after drying;
Step b: 0.07L Oleum Anisi Stellati is dissolved in ethanol, preparation 65%(volume ratio) Oleum Anisi Stellati alcoholic solution, and by 0.77kg β-CD water-soluble preparation β-CD saturated solution at 60 DEG C, then at 40 DEG C, the Oleum Anisi Stellati alcoholic solution of preparation is mixed with β-CD saturated solution, stir under 850r/min and obtain milky suspension in 2 hours, described milky suspension is left standstill 24 hours at 4 DEG C, white precipitate is obtained after filtration, by described white precipitate at 45 DEG C of low-temperature vacuum drying baking oven (ZDF-15, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing) in dry 2-3h, after most of moisture is volatilized, then at 45 DEG C of heated-air circulation oven (GT-G-II, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing) middle placement 5h, obtain Oleum Anisi Stellati clathrate,
Step c: the Oleum Anisi Stellati clathrate obtained in step b is mixed with the granule obtained in step a, through soft material processed, granulate and (adopt oscillating granulator (YK-160, Feilong Pharmaceutical Machinery Equipment Factory, Nanjing)) after obtain wet granular, dry described wet granular at 60 DEG C, sieve after granulate and obtain dry granule, described dry granule is mixed with 0.2kg film coating powder, adopt rotary tablet machine (ZPY-23E, Shanghai Jiangnan Pharmaceutical Machinary Co., Ltd) tabletting is carried out to described dry granule, and adopt high-efficiency coating machine (BG-80, king's pharmaceutical machine Equipment Limited, sea, Nanjing) coating is carried out to described granule, obtain glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet 7.
The yield of the Oleum Anisi Stellati clathrate prepared according to following formulae discovery above-described embodiment 1-7, envelop rate and comprehensive grading, result of calculation is as shown in table 1.
Comprehensive grading=envelop rate × 80%+ clathrate yield × 20%
Oleum Anisi Stellati clathrate performance parameter in table 1 embodiment 1-7
As seen from Table 1, the envelop rate comprehensive grading of clathrate prepared by above-described embodiment 1-7 is all more than 81%, tablet product qualified rate is all greater than 80%, especially the comprehensive grading of the glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet of embodiment 3 and 7 preparation reaches more than 92%, show that the preparation method of glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet of the present invention meets " Chinese Pharmacopoeia " 2010 editions two pertinent regulations, actual production and industrialized needs can be met.
comparative example
Adopt existing method to prepare glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet, wherein each amounts of components is identical with consumption corresponding in embodiment 1.Concrete preparation method is as follows:
Step 1: adopt the method for embodiment 1 to prepare Bulbus Fritillariae Thunbergii fluid extract, Radix Platycodonis fluidextract, Radix Polygalae fluid extractum, Radix Glycyrrhizae extractum fine powder, Radix Glycyrrhizae fluidextract;
Step 2: prepare granule according to the method in embodiment 1 step a;
Step 3: granule Oleum Anisi Stellati and step 2 prepared mixes; wet granular is obtained after soft material processed, granulation; dry described wet granular at 60 DEG C; sieve after granulate and obtain dry granule; described dry granule is mixed with 0.38kg film coating powder; adopt rotary tablet machine to carry out tabletting to described dry granule, and adopt high-efficiency coating machine to carry out coating to described granule, obtain glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet.
test 1: glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet performance test
Character observation: the glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet prepared in above-described embodiment 1-7 is Film coated tablets, aobvious light brown after removing coating, tablet is complete bright and clean, uniform color, and hardness is moderate.
Medicine performance checking and mensuration: rise International Country drug standard the 4th detect the weight differential of the glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet prepared of embodiment 1-7, disintegration, ammonium chloride and glycyrrhizic acid content according to chemical drugs, test result is as shown in table 2.
Table 2: the performance detection data of the glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet prepared in embodiment 1-7
In above-mentioned table 2, the concrete meaning of each test item is as follows:
Differentiate that (1) represents: in test sample chromatograph, on the position corresponding to Radix Polygalae control medicinal material chromatograph, the speckle of aobvious same color, be then judged to and conform with the regulations, otherwise be judged to against regulation.
Differentiate that (2) represent: in test sample chromatograph, on the position corresponding to Bulbus Fritillariae Thunbergii control medicinal material chromatograph, the speckle of aobvious same color, be then judged to and conform with the regulations, otherwise be judged to against regulation.
Weight differential: be judged in 0.6 ± 0.03g and conform with the regulations.
Disintegration: if whole disintegrate within 60 minutes, be then judged to and conform with the regulations.
Ammonium chloride content %: refer to that in tablet, the actual content of ammonium chloride accounts for the ratio of ammonium chloride theoretical content.
As seen from Table 2, the related request during the national drug standards that all meet the glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet adopting the inventive method to prepare detect.
test 2: clathrate stability test
According to " Chinese Pharmacopoeia " version determination of volatile oil method in 2010, Oleum Anisi Stellati clathrate prepared by above-described embodiment 1-7 38-42 DEG C, relative humidity carries out oil content detection under being the condition of 70-80%, test respectively Oleum Anisi Stellati clathrate 1,2,3, oil content (Fructus Anisi Stellati weight of oil accounts for the percentage ratio of clathrate weight) after June.
Table 3: embodiment of the present invention 1-7 stability of volatile oil is tested
As seen from Table 3, after high temperature experiment, adopt the Fructus Anisi Stellati oil content of clathrate in the glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet prepared of the inventive method 1,2,3, all there is not significant change after June, the glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet that explanation the present invention adopts clathrate process to prepare thus can improve the stability of volatile oil, extend volatile oil retention time, thus the stability of medicine can be improved.
test 3: stability of volatile oil test in medicament
Respectively under high temperature and room temperature, the stability of glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet prepared by investigation above-described embodiment 1-7 and comparative example.High temperature test condition is as follows: be under the condition of 60 ± 10% at relative humidity, above-mentioned glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet is placed 10 days in 40 DEG C and 60 DEG C of calorstats, interval different time sampling, measure volatile oil content (in units of ml/100g sample) by " Chinese Pharmacopoeia " 2005 editions one annex XD determination of volatile oil Division A League Matches of French Football method (annex 57 pages), measurement result is as shown in table 4 and table 5.Room temperature test condition is as follows: be under the condition of 60 ± 10% at relative humidity, above-mentioned glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet is placed 3 months at 25 ± 2 DEG C, interval different time sampling, measure volatile oil content (in units of ml/100g sample) by " Chinese Pharmacopoeia " 2005 editions one annex XD determination of volatile oil Division A League Matches of French Football method (annex 57 pages), measurement result is as shown in table 6.
Stability of volatile oil test in medicament at table 440 DEG C
Stability of volatile oil test in medicament at table 560 DEG C
Stability of volatile oil test in medicament under table 6 room temperature
Find out from table 4 to table 6, the glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet prepared of the embodiment of the present invention at high temperature (40 DEG C, 60 DEG C) and ambient temperatare is put time, in tablet, Fructus Anisi Stellati oil content remains unchanged substantially, and the glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet adopting existing method to prepare at high temperature (40 DEG C, 60 DEG C) and ambient temperatare is put time, in tablet, Fructus Anisi Stellati oil content reduces gradually.Illustrate thus, relative to prior art, the present invention adopts microcapsule technology to prepare glycyrrhiza compound Bulbus Fritillariae Thunbergii ammonium chloride tablet, is conducive to the stability improving volatile oil, thus improves the stability of medicine.
Specific description of embodiments of the present invention does not above limit the present invention, and those skilled in the art can make various change or distortion according to the present invention, only otherwise depart from spirit of the present invention, all should belong to the scope of claims of the present invention.
Claims (19)
1. a compound liquorice-fritillarithunbergii-ammonium thunbergii-ammonium chloride medicinal composition, this pharmaceutical composition comprises:
Wherein, described Oleum Anisi Stellati and described beta-schardinger dextrin-form clathrate, and described parts by volume and weight ratio are ml/g or L/kg;
Wherein, the method that described Oleum Anisi Stellati and beta-schardinger dextrin-form clathrate comprises the following steps:
Get Oleum Anisi Stellati and add the Oleum Anisi Stellati alcoholic solution that ethanol is mixed with 65% volume ratio, by water-soluble for beta-schardinger dextrin-preparation β-CD saturated solution at 56-60 DEG C, at 40 DEG C, Oleum Anisi Stellati alcoholic solution is mixed with beta-schardinger dextrin-saturated solution, stir under 850 revs/min and obtain milky suspension in 2 hours, described milky suspension is left standstill 24-36 hour at 2-6 DEG C, white precipitate is obtained after filtration, by described white precipitate dry 3-8 hour at 45 DEG C, obtain described Oleum Anisi Stellati clathrate.
2. pharmaceutical composition according to claim 1, is characterized in that, described pharmaceutical composition comprises:
3. pharmaceutical composition according to claim 1, is characterized in that, described pharmaceutical composition comprises:
4. pharmaceutical composition according to any one of claim 1 to 3, is characterized in that, is formed in the method for clathrate at described Oleum Anisi Stellati and beta-schardinger dextrin-, by water-soluble for beta-schardinger dextrin-preparation β-CD saturated solution at 60 DEG C.
5. pharmaceutical composition according to any one of claim 1 to 3, is characterized in that, is formed in the method for clathrate at described Oleum Anisi Stellati and beta-schardinger dextrin-, and described milky suspension is left standstill 24-36 hour at 4 DEG C.
6. pharmaceutical composition according to any one of claim 1 to 3, is characterized in that, is formed in the method for clathrate at described Oleum Anisi Stellati and beta-schardinger dextrin-, and described milky suspension is left standstill 24 hours at 2-6 DEG C.
7. pharmaceutical composition according to any one of claim 1 to 3, is characterized in that, is formed in the method for clathrate at described Oleum Anisi Stellati and beta-schardinger dextrin-, and described milky suspension is left standstill 24 hours at 4 DEG C.
8. pharmaceutical composition according to any one of claim 1 to 3, it is characterized in that, formed in the method for clathrate at described Oleum Anisi Stellati and beta-schardinger dextrin-, by the described white precipitate first dry 2-3h in 45 DEG C of low-temperature vacuum drying baking ovens obtained after filtration, after most of moisture is volatilized, then in 45 DEG C of heated-air circulation ovens, place 5h, obtain described Oleum Anisi Stellati clathrate.
9. pharmaceutical composition according to any one of claim 1 to 3, is characterized in that, described pharmaceutical composition is tablet, capsule or granule.
10. pharmaceutical composition according to claim 9, is characterized in that, described pharmaceutical composition is tablet.
11. pharmaceutical compositions according to any one of claim 1 to 3, is characterized in that, described pharmaceutical composition also comprises pharmaceutically acceptable adjuvant.
12. pharmaceutical compositions according to claim 11, is characterized in that, described pharmaceutical composition also comprises:
13. pharmaceutical compositions according to any one of claim 1 to 3, is characterized in that, the preparation method of described Radix Polygalae fluid extractum comprises the following steps:
Radix Polygalae powder is broken into 65 orders, solvent is made with the ethanol water of 60% volume ratio, flood after 24 hours, the speed of dividing with 1-3ml/ carries out percolation, collect the first liquid of filtering of 85%, another extracting container preserves liquid of just filtering, continue percolation, after soluble component is filtered out completely, collection is filtered liquid, and below 60 DEG C cryoconcentration to paste, add the initial first liquid of filtering preserved, mixing, drip concentrated ammonia solution and make the micro-aobvious alkalescence of filtrate, and have ammonia smelly, then crude drug weight is diluted to the ethanol water of 60% volume ratio, make the fluid extract that ethanol content is 38-48% volume ratio, leave standstill, filter after clarification and obtain described Radix Polygalae fluid extractum.
14. pharmaceutical compositions according to claim 13, is characterized in that, the preparation method of described Radix Polygalae fluid extractum comprises the following steps:
Radix Polygalae powder is broken into 65 orders, solvent is made with the ethanol water of 60% volume ratio, flood after 24 hours, the speed of dividing with 1-3ml/ carries out percolation, collect the first liquid of filtering of 85%, another extracting container preserves liquid of just filtering, continue percolation, after soluble component is filtered out completely, collection is filtered liquid, and below 60 DEG C cryoconcentration to paste, add the initial first liquid of filtering preserved, mixing, the concentrated ammonia solution dripping 25-28% volume ratio makes the pH value of filtrate be 9-10, then crude drug weight is diluted to the ethanol water of 60% volume ratio, make the fluid extract that ethanol content is 38-48% volume ratio, leave standstill, filter after clarification and obtain described Radix Polygalae fluid extractum.
15. pharmaceutical compositions according to any one of claim 1 to 3, is characterized in that, the preparation method of described Bulbus Fritillariae Thunbergii fluid extract comprises the following steps:
Bulbus Fritillariae Thunbergii is ground into 24 orders, solvent is made with the ethanol water of 70% volume ratio, flood after 18 hours, the speed of dividing with 1-3ml/ carries out percolation, collect the first liquid of filtering of 85%, another extracting container preserves liquid of just filtering, continue percolation, after soluble component is filtered out completely, by remaining filter liquid below 60 DEG C low-temperature evaporation to paste, add the initial first liquid of filtering preserved, mixing, the ethanol water adding 70% volume ratio is again diluted to crude drug weight, make the fluid extract that ethanol content is 50-70% volume ratio, mixing, leave standstill, described Bulbus Fritillariae Thunbergii fluid extract is obtained after filtration.
16. pharmaceutical compositions according to any one of claim 1 to 3, is characterized in that, the preparation method of described Radix Platycodonis fluidextract comprises the following steps:
Balloonflower powder is broken into 24 orders, solvent is made with the ethanol water of 55% volume ratio, flood after 48 hours, the slow percolation of the speed of dividing with 1-3ml/, collect the first liquid of filtering of 85%, another extracting container preserves liquid of just filtering, and continues percolation, after soluble component is filtered out completely, by remaining filter liquid below 60 DEG C low-temperature evaporation to paste, add the initial first liquid of filtering preserved, mixing, then the ethanol water adding 55% volume ratio is diluted to crude drug weight, make the fluid extract that ethanol content is 40-50% volume ratio, mixing, leaves standstill, obtains described Radix Platycodonis fluidextract after filtration.
17. pharmaceutical compositions according to any one of claim 1 to 3, is characterized in that, the preparation method of described Radix Glycyrrhizae extractum powder comprises the following steps:
By Radix Glycyrrhizae extracting in water three times, each 2 hours, merge extractive liquid, placed extracting solution and spends the night, extracting solution is precipitated, then gets supernatant concentration to paste, crushed after being dried to 80 order, obtain described Radix Glycyrrhizae extractum powder.
18. pharmaceutical compositions according to any one of claim 1 to 3, is characterized in that, the preparation method of described Radix Glycyrrhizae fluidextract comprises the following steps:
(1) by Radix Glycyrrhizae extracting in water three times, each 2 hours, merge extractive liquid, placed extracting solution and spends the night, extracting solution is precipitated, then gets supernatant concentration to paste, crushed after being dried to 80 order, obtain described Radix Glycyrrhizae extractum powder;
(2) by described Radix Glycyrrhizae extractum powder, with the ethanol extraction three times of 92% volume ratio, merge extractive liquid, reclaim ethanol, the ethanol dilution adding suitable quantity of water and 92% volume ratio, to crude drug weight, makes the Radix Glycyrrhizae fluidextract that ethanol content is 20-25% volume ratio.
The preparation method of 19. pharmaceutical compositions according to any one of claim 1 to 18, this preparation method comprises the following steps:
Step a: Radix Polygalae fluid extractum, Bulbus Fritillariae Thunbergii fluid extract, Radix Platycodonis fluidextract, Radix Glycyrrhizae fluidextract, Radix Glycyrrhizae extractum, ammonium chloride, calcium carbonate, starch and dextrin mixed, mixes thoroughly, make granule after drying;
Step b: Oleum Anisi Stellati is mixed with the granule that step a obtains with the clathrate of beta-schardinger dextrin-;
Then, the mixture obtained to step b adds pharmaceutically acceptable adjuvant, and after soft material processed, granulation, obtain wet granular, at 60 DEG C, dry described wet granular, obtains dry granule after the granulate that sieves, and carries out tabletting, coating to described dry granule, obtained tablet.
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| CN1562307A (en) * | 2004-04-09 | 2005-01-12 | 甘肃甘帝制药有限公司 | Method for preparing compound licorice buccal tablet |
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2013
- 2013-11-28 CN CN201310629709.3A patent/CN103690759B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1562307A (en) * | 2004-04-09 | 2005-01-12 | 甘肃甘帝制药有限公司 | Method for preparing compound licorice buccal tablet |
Non-Patent Citations (4)
| Title |
|---|
| 八角茴香油β-环糊精包合物的稳定性考察;黄德凤等;《广西中医药》;20100831;第33卷(第4期);第58-59页 * |
| 复方甘草浙贝氯化铵片;国家药典委员会编;《化学药品地标升国标国家药品标准第4册》;20021231;第164页 * |
| 桔梗流浸膏;奚念朱主编;《药剂学》;人民卫生出版社;19960430;第44页 * |
| 甘草流浸膏、甘草浸膏、远志流浸膏、浙贝流浸膏;国家药典委员会编;《中华人民共和国药典2010年版》;中国医药科技出版社;20100131;第376、380、390页 * |
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| CN103690759A (en) | 2014-04-02 |
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