CN1276779C - Hollow capsule material composition of plant polysaccharide and production of hollow capsule - Google Patents
Hollow capsule material composition of plant polysaccharide and production of hollow capsule Download PDFInfo
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- CN1276779C CN1276779C CN 200510079888 CN200510079888A CN1276779C CN 1276779 C CN1276779 C CN 1276779C CN 200510079888 CN200510079888 CN 200510079888 CN 200510079888 A CN200510079888 A CN 200510079888A CN 1276779 C CN1276779 C CN 1276779C
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- 239000000203 mixture Substances 0.000 title claims abstract description 83
- 239000002775 capsule Substances 0.000 title claims abstract description 81
- 150000004676 glycans Chemical class 0.000 title claims description 31
- 229920001282 polysaccharide Polymers 0.000 title claims description 31
- 239000005017 polysaccharide Substances 0.000 title claims description 31
- 239000000463 material Substances 0.000 title claims description 20
- 238000004519 manufacturing process Methods 0.000 title description 15
- 229920001525 carrageenan Polymers 0.000 claims abstract description 67
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000003292 glue Substances 0.000 claims abstract description 61
- 239000000679 carrageenan Substances 0.000 claims abstract description 50
- 229940113118 carrageenan Drugs 0.000 claims abstract description 50
- 229920002678 cellulose Polymers 0.000 claims abstract description 27
- 239000001913 cellulose Substances 0.000 claims abstract description 27
- 238000002360 preparation method Methods 0.000 claims abstract description 26
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 239000011347 resin Substances 0.000 claims abstract description 22
- 229920005989 resin Polymers 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000004090 dissolution Methods 0.000 claims abstract description 19
- 238000005520 cutting process Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000007598 dipping method Methods 0.000 claims abstract description 8
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 120
- 229920002472 Starch Polymers 0.000 claims description 76
- 235000019698 starch Nutrition 0.000 claims description 76
- 239000008107 starch Substances 0.000 claims description 72
- 238000000034 method Methods 0.000 claims description 37
- 230000008569 process Effects 0.000 claims description 35
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims description 33
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 32
- 229920003163 Eudragit® NE 30 D Polymers 0.000 claims description 29
- 235000013311 vegetables Nutrition 0.000 claims description 29
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 28
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 28
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 26
- 235000010980 cellulose Nutrition 0.000 claims description 26
- 239000011734 sodium Substances 0.000 claims description 26
- 229910052708 sodium Inorganic materials 0.000 claims description 26
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 21
- 229960003943 hypromellose Drugs 0.000 claims description 21
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 20
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 20
- 240000008042 Zea mays Species 0.000 claims description 19
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 19
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 19
- 150000001298 alcohols Chemical class 0.000 claims description 19
- 229920001577 copolymer Polymers 0.000 claims description 19
- 235000005822 corn Nutrition 0.000 claims description 19
- 241001597008 Nomeidae Species 0.000 claims description 15
- 238000006116 polymerization reaction Methods 0.000 claims description 15
- 239000004925 Acrylic resin Substances 0.000 claims description 13
- 102220289725 rs778831047 Human genes 0.000 claims description 12
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 claims description 10
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 claims description 10
- GDCRSXZBSIRSFR-UHFFFAOYSA-N ethyl prop-2-enoate;2-methylprop-2-enoic acid Chemical compound CC(=C)C(O)=O.CCOC(=O)C=C GDCRSXZBSIRSFR-UHFFFAOYSA-N 0.000 claims description 9
- 229920001353 Dextrin Polymers 0.000 claims description 8
- 239000004375 Dextrin Substances 0.000 claims description 8
- 235000019425 dextrin Nutrition 0.000 claims description 8
- 239000001863 hydroxypropyl cellulose Substances 0.000 claims description 8
- 229920003134 Eudragit® polymer Polymers 0.000 claims description 7
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 7
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 6
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 6
- 239000001856 Ethyl cellulose Substances 0.000 claims description 6
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 6
- 229920003135 Eudragit® L 100-55 Polymers 0.000 claims description 6
- 229910001424 calcium ion Inorganic materials 0.000 claims description 6
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 6
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 6
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 6
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 6
- 229920001249 ethyl cellulose Polymers 0.000 claims description 6
- 229910001414 potassium ion Inorganic materials 0.000 claims description 6
- 229920003151 Eudragit® RL polymer Polymers 0.000 claims description 5
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 5
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 claims description 5
- -1 dimethylaminoethyl Chemical group 0.000 claims description 5
- DNKKLDKIFMDAPT-UHFFFAOYSA-N n,n-dimethylmethanamine;2-methylprop-2-enoic acid Chemical compound CN(C)C.CC(=C)C(O)=O.CC(=C)C(O)=O DNKKLDKIFMDAPT-UHFFFAOYSA-N 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 5
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 5
- 229920003149 Eudragit® E 100 Polymers 0.000 claims description 3
- NEDGUIRITORSKL-UHFFFAOYSA-N butyl 2-methylprop-2-enoate;2-(dimethylamino)ethyl 2-methylprop-2-enoate;methyl 2-methylprop-2-enoate Chemical compound COC(=O)C(C)=C.CCCCOC(=O)C(C)=C.CN(C)CCOC(=O)C(C)=C NEDGUIRITORSKL-UHFFFAOYSA-N 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims 1
- 239000003814 drug Substances 0.000 abstract description 13
- 238000001035 drying Methods 0.000 abstract description 5
- 241000196324 Embryophyta Species 0.000 description 18
- 230000002496 gastric effect Effects 0.000 description 16
- 235000010418 carrageenan Nutrition 0.000 description 12
- 108010010803 Gelatin Proteins 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 10
- 239000008273 gelatin Substances 0.000 description 10
- 229920000159 gelatin Polymers 0.000 description 10
- 235000019322 gelatine Nutrition 0.000 description 10
- 235000011852 gelatine desserts Nutrition 0.000 description 10
- 239000007902 hard capsule Substances 0.000 description 9
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical group [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 9
- LUEWUZLMQUOBSB-FSKGGBMCSA-N (2s,3s,4s,5s,6r)-2-[(2r,3s,4r,5r,6s)-6-[(2r,3s,4r,5s,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5s,6r)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-4,5-dihydroxy-2-(hydroxymethyl)oxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound O[C@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@@H](O[C@@H]2[C@H](O[C@@H](OC3[C@H](O[C@@H](O)[C@@H](O)[C@H]3O)CO)[C@@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O LUEWUZLMQUOBSB-FSKGGBMCSA-N 0.000 description 7
- 229920002752 Konjac Polymers 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- 241001465754 Metazoa Species 0.000 description 6
- 239000000499 gel Substances 0.000 description 6
- 238000005189 flocculation Methods 0.000 description 5
- 230000016615 flocculation Effects 0.000 description 5
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- 108010073771 Soybean Proteins Proteins 0.000 description 4
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 235000018102 proteins Nutrition 0.000 description 4
- 108090000623 proteins and genes Proteins 0.000 description 4
- 102000004169 proteins and genes Human genes 0.000 description 4
- 235000019710 soybean protein Nutrition 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- 208000007212 Foot-and-Mouth Disease Diseases 0.000 description 3
- 241000710198 Foot-and-mouth disease virus Species 0.000 description 3
- 208000018756 Variant Creutzfeldt-Jakob disease Diseases 0.000 description 3
- 208000005881 bovine spongiform encephalopathy Diseases 0.000 description 3
- 159000000007 calcium salts Chemical class 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- 239000012744 reinforcing agent Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 239000000080 wetting agent Substances 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 229920003139 Eudragit® L 100 Polymers 0.000 description 2
- 210000000988 bone and bone Anatomy 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 235000011148 calcium chloride Nutrition 0.000 description 2
- 239000000701 coagulant Substances 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 229920000609 methyl cellulose Polymers 0.000 description 2
- 239000001923 methylcellulose Substances 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 239000001508 potassium citrate Substances 0.000 description 2
- 229960002635 potassium citrate Drugs 0.000 description 2
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 description 2
- 235000011082 potassium citrates Nutrition 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- 229920001661 Chitosan Polymers 0.000 description 1
- 208000035473 Communicable disease Diseases 0.000 description 1
- 108010082495 Dietary Plant Proteins Proteins 0.000 description 1
- STECJAGHUSJQJN-GAUPFVANSA-N Hyoscine Natural products C1([C@H](CO)C(=O)OC2C[C@@H]3N([C@H](C2)[C@@H]2[C@H]3O2)C)=CC=CC=C1 STECJAGHUSJQJN-GAUPFVANSA-N 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- STECJAGHUSJQJN-UHFFFAOYSA-N N-Methyl-scopolamin Natural products C1C(C2C3O2)N(C)C3CC1OC(=O)C(CO)C1=CC=CC=C1 STECJAGHUSJQJN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 239000004141 Sodium laurylsulphate Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 230000037213 diet Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 235000013376 functional food Nutrition 0.000 description 1
- 210000004211 gastric acid Anatomy 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 230000000968 intestinal effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 229940127557 pharmaceutical product Drugs 0.000 description 1
- 229960003975 potassium Drugs 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 108010091872 satietin Proteins 0.000 description 1
- STECJAGHUSJQJN-FWXGHANASA-N scopolamine Chemical compound C1([C@@H](CO)C(=O)O[C@H]2C[C@@H]3N([C@H](C2)[C@@H]2[C@H]3O2)C)=CC=CC=C1 STECJAGHUSJQJN-FWXGHANASA-N 0.000 description 1
- 229960002646 scopolamine Drugs 0.000 description 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 1
- 229940126589 solid medicine Drugs 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/4816—Wall or shell material
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Medicinal Preparation (AREA)
Abstract
The present invention relates to a hollow capsule used in medicine and a preparation method for the hollow capsule. The raw-material composition of the hollow capsule contains (by weight ratio) 0.5 to 26 portions of K-carrageenan, 75 to 98 portions of cellulose derivative and/or resin and 1 to 12 portions of alcohol. In the preparation method, all the raw materials are put into a reaction vessel except alcohol, and then water is added; alcohol is added in the course of dissolution of the raw materials, then glue solution forms, and after glue dipping, drying, defilming, cutting and sheathing, the hollow capsule forms. The hollow capsule prepared by the present invention is stable in performance and long in shelf life, and all categories of quality indexes of the hollow capsule are completely in accord with the specification of the Pharmacopoeia of Peoples Republic of China of the current edition and/or the national standard.
Description
Technical field
The present invention relates to a kind of pharmaceutical product, a kind of Capsules that is used for fill graininess, powdered solid medicine, functional food, health product and cosmetics and preparation method thereof of more specifically saying so.
Background technology
The hollow and hard capsule is existing for a long time as the application of pharmaceutical carrier.The hollow and hard capsule is a raw material with gelatin generally, adds water and makes.Used production method is that gelatin is soaked, expanded, and stirs in reaction pot, dissolves, and the temperature of reaction pot remains on 60-75 ℃; After the dissolving glue is filtered, regulate gelatin concentration, store insulation, peeling removes bubble, forms finished product dipping in automatically on the glue production line through dipping in glue, oven dry, cooling, demoulding, cutting, fit, check, packing.
Because the raw material sources of gelatin are in skin, the bone of animal, gelatin is the animal proteinum colloid, and contains the animal little fat.After making Capsules with the gelatin of the skin of some animal, bone system, the people of faith Islam, kosher can't take.On the other hand, because animality infectious disease from spreading such as European bovine spongiform encephalopathy, foot and mouth disease have caused the safety problem of using.
And, comparatively responsive with the Capsules that gelatin is made to temperature and humidity.With the medicine that its Capsules of making is packed, be preferably under the condition of constant humidity and store.Humidity is too high, the easy softening transform of capsule; The easy embrittlement of capsule under the low excessively condition of humidity.And gelatin easily reacts with the medicine that contains aldehyde radical and tannin, produces insoluble substance, and the capsule disintegration time is prolonged, and the capsule color changes.
Because with gelatin is that the capsule that raw material is made exists above-mentioned weak point, it is in the research of feedstock production Capsules that the researcher of this respect has focused on attention with vegetable polysaccharides.
The Chinese patent literature application number is that 200410012944.7 (applying date is on March 30th, 2004, and open day is on January 12nd, 2005, and publication number is CN1561971A) disclose a kind of plant hollow and hard capsule, and it is made by following raw materials by weight percent; Modified konjaku glucomannoglycan 31%-51%, soybean protein isolate 25.4%-47.8%, coagulant are 8.8%-27.5%, and flocculation aid is 3.3%-7%, and water is 3.4%-9%; The modified konjaku glucomannoglycan is carboxy methyl konjaku glucomannoglycan, oxidation glucomannoglycan, maleic anhydride esterification glucomannoglycan, acetic anhydride esterification glucomannoglycan; Coagulant is carrageenan or yellow source glue; Flocculation aid is for providing cation Ca
2+, K
+Salt such as potassium chloride, potassium citrate, potassium phosphate, calcium chloride.
Its preparation method is may further comprise the steps:
A) with Rhizoma amorphophalli powder gelatinizing under 40-70 ℃ of temperature, add konjaku powder 10wt%-120wt% modifier, reacted 2-4 hour, washing, drying and crushing gets the modified konjaku glucomannoglycan.
B) with soybean protein isolate dispersed with stirring under 30-60 ℃ of temperature, the soybean protein isolate solids content is 1-8%, 80-100 ℃ heat treatment 25-35 minute, the accent pH value is 9-10.
C) modified product of the konjaku powder of adding soybean protein isolate 65wt%-200wt% and the cross-linking agent of dry powder total amount 0.01%-10%, under 40-70 ℃ of temperature copolyreaction 2-5 hour, the washing, drying, pulverize modified konjaku glucomannoglycan-soybean protein isolate complex.
D) under 60-80 ℃ of temperature with CMGM-SPI complex colloidal sol, add coagulation system, stir, after the insulation de-bubbled, pour feed liquid into immersion trough, dip in glue, oven dry, promptly can be made into plant hollow and hard capsule after dialling shell, cutting and arrangement through transverse slat again.
This invention need not storage at a constant temperature; All be plant material, can not propagate foot and mouth disease and bovine spongiform encephalopathy, be difficult for polluting, satietin diet culture person's requirement is suitable for containing the storage and the transportation of aldehyde radical medicine.But also there is weak point.Because having added potassium salt has influenced disintegration, has added protein microorganism is exceeded standard easily, also be not easy to store.
Another piece Chinese patent literature application number is that 20031010801.2 (applying date is on October 15th, 2003, and open day is on April 20th, 2005) disclose a kind of plant hollow capsule and production technology thereof.The proportioning of its glue is as follows: plant gum 16-25%, reinforcing agent 2.0-5.0%, surfactant 0.02%-0.026%, wetting agent 0.15%-0.20%, surplus are water.Described plant gum is a kind of in pectin, the carrageenan or two kinds, and described reinforcing agent is one or more in chitosan, carboxymethyl starch, the hydroxypropyl cellulose, and described surfactant is a sodium lauryl sulphate, and described wetting agent is a glycerol.
The production technology of its preparation Capsules is: the percetage by weight ratio by each component is got the raw materials ready, earlier plant gum is soaked expansion, putting into reaction pot stirs, dissolves, add reinforcing agent, surfactant and wetting agent during this time, and in the reaction pot interlayer, feed 50 ℃-85 ℃ recirculated water, treat that fully glue is filtered with the 100-120 order in the dissolving back, be stored in the heat-preserving container, regulate gelatin concentration during use, peeling removes bubble, is dipping in automatically on the glue production line through dipping in glue, oven dry, cooling, demoulding, cutting, fit, check, packing.
With the plant hollow hard capsule that the batching and the production technology of this invention are produced, good stability, indeformable under high temperature or high humidity environment, embrittlement is not convenient to permanent storage.In this technology, also do not add potassium salt, calcium salt, but the proportioning of each component is not suitable for, disintegration time is prolonged, be difficult to meet the quality standard of current edition Pharmacopoeia of the People's Republic of China defined.
One piece of Chinese patent literature application number is 99116921.2 (applying date is JIUYUE in 1999 28 days, and open day is April 25 calendar year 2001, and publication number is CN1292261A) discloses another plant hard capsule and production technology thereof again.This plant hard capsule is made up of hydrophilic gel, water-soluble cellulose, flocculation aid and water, their weight percentages of components is: hydrophilic gel 0.01%-11.87%, water-soluble cellulose 71.25%-94.8%, help gel 0.10%-11.87%, water 5%-8%.
Said hydrophilic gel can be K type carrageenan, and flocculation aid is potassium chloride, calcium chloride, calcium phosphate, potassium citrate.
Its production technology is: the water of pouring 60%-89.98% in percentage by weight is the flocculation aid of the hydrophilic gel of 0.01%-5% and 0.01%-5% into, stir, be heated to more than 80 ℃, to the colloid uniform dissolution, again the water-soluble cellulose of 10%-30% poured into, dried, promptly can be made into after dialling shell, cutting and arrangement.
The plant hollow hard capsule that utilizes this invention to prepare, in soak after 10 days, indeformable, because used raw material is mainly vegetable polysaccharides, protein and fat content low (being respectively 0.5% and 0.3%), and make vegetable protein and plant fat, avoided the pollution that may cause by animal proteinum.Though the amount of the K-carrageenan that its weak point is used is lower, but potassium salt or calcium salt have been added, the K-carrageenan potassium salt or the calcium salt that form, make capsular disintegration elongated, reach 15-16.5min, do not meet the requirement of existing Chinese Pharmacopoeia standard, the current edition Pharmacopoeia of the People's Republic of China require its under one's belt disintegration be within 10 minutes.
Summary of the invention
Purpose of the present invention just is to work out a kind of vegetable polysaccharides Capsules feedstock composition, the Capsules that uses this feedstock composition to go out as feedstock production, overcome the capsular deficiency that prior art is made, indeformable under high temperature, high humidity or cold environment, embrittlement not, good stability, be convenient to long term store, can meet the regulation of the current edition Pharmacopoeia of the People's Republic of China and/or national standard its disintegration again.
Another object of the present invention works out exactly and utilizes above-mentioned a kind of vegetable polysaccharides Capsules feedstock composition to be raw material, prepares the preparation method that function admirable meets the Capsules of Pharmacopoeia of the People's Republic of China standard.
In order to work out a kind of vegetable polysaccharides Capsules material combination composition formula, various exploitative experiments have been carried out.Once with K-carrageenan and the 0.3%-4.5% percetage by weight potassium ion and/or the calcium ion of the percetage by weight of the hypromellose 0.1%-4% of 81%-97.5% percetage by weight, prepared a kind of Capsules, find that after tested disintegration is long, do not meet the requirement of disintegration of existing China national pharmacopeia.This may be to have prolonged event disintegration owing to having added potassium or calcium ion.
For this reason, through deep experimental studies have found that, mix by proper proportion by vegetable polysaccharides, cellulose derivative and/or resin, starch and derivant thereof, alcohols, form vegetable polysaccharides Capsules feedstock composition, by the controlling plant polysaccharide is exactly the consumption of control K-carrageenan and the consumption of other compositions, can make the molten diffusing vegetable polysaccharides Capsules of easy disintegrating.
A kind of vegetable polysaccharides Capsules feedstock composition of the present invention comprises K-carrageenan 0.5-26 weight portion, cellulose derivative and/or resin 75-98 weight portion, alcohols 1-12 weight portion.
Said cellulose derivative is wherein a kind of of hypromellose, ethyl cellulose, hydroxypropyl cellulose, carboxymethyl cellulose or wherein arbitrarily two kinds of weight ratio;
Said resin is wherein a kind of of polyvinyl alcohol, polyacrylic resin, polyvidone or wherein arbitrarily two kinds of weight ratio; Above-mentioned polyvinyl alcohol is PVAC polyvinylalcohol-0588 or PVAC polyvinylalcohol-1788, and its degree of polymerization is respectively 500 and 1700; Above-mentioned polyacrylic resin is EUDRAGIT NE 30 D EUDRAGIT NE 30D Eudragit E30D, dimethylaminoethyl methacrylate-neutral methacrylic acid esters copolymer EudragitE100, methacrylic acid-methyl acrylate copolymer EudragitL100-55, neutral EUDRAGIT NE 30 D EUDRAGIT NE 30D Eudragit NE30D, methacrylic acid three ammoniums ethyl ester-acrylate copolymer Eudragit RL;
Said alcohols is ethanol, the glycerol a kind of or ethanol wherein and the mixture of any weight ratio of glycerol;
Said composition does not contain potassium ion or calcium ion.
In order to quicken disintegrate, add starch and derivant 1-15 weight portion thereof for well.Form K-carrageenan 0.5-26 weight portion, cellulose derivative and/or resin 75-98 weight portion, the plant hollow capsule feedstock composition of alcohols 1-12 weight portion starch and derivant 1-15 weight portion thereof.
In feedstock composition, add resin formation and contain the feedstock composition that does not have cellulose derivative that fiber derivative contains the feedstock composition of resin again or only contains resin, be in order to change capsular disintegrating property, requirement according to medicine, the rate of release of control medicine, make the Capsules of producing insoluble under one's belt, and it is molten diffusing at enteral, control its in 60 minutes in the enteral disintegrate, so sometimes, can avoid some medicine to be decomposed by gastric acid to the stimulation of stomach or at gastric destroys, make it again after the enteral disintegrate, absorbed by intestinal, increased medicine the treatment of diseases effect.The cellulose derivative that is added and/or the amount of resin are the 75-98 weight portion, are advisable with the 90-96 weight portion again.
In order to make the Capsules for preparing have more performance, in feedstock composition, add polyvinyl alcohol, the amount that makes the mixture of polyvinyl alcohol and cellulose derivative is the 75-98 weight portion, forming K-carrageenan 0.5-26 weight portion, cellulose derivative and polyvinyl alcohol mixture is the 75-98 weight portion, the feedstock composition of alcohols 1-12 weight portion, starch and derivant 1-15 weight portion thereof, the fiber derivative that is added and the amount of polyvinyl alcohol are advisable with the 90-96 weight portion again.Cellulose derivative and polyvinyl alcohol be the mixture of weight ratio arbitrarily, is 1: 1～3 for good with the weight ratio of polyvinyl alcohol and cellulose derivative again, and the degree of polymerization of used polyvinyl alcohol is 500-1700.
The K-carrageenan is the 0.5-26 weight portion in above-mentioned all feedstock compositions, and is for well, better with 2.3-＜4.2 weight portions with the 2-10 weight portion.If the amount of used carrageenan greater than 26 weight portions, makes its disintegration time at gastric prolong.
Said cellulose derivative can be wherein a kind of of hypromellose, ethyl cellulose, hydroxypropyl cellulose, carboxymethyl cellulose or wherein arbitrarily two kinds of weight ratio.
Said resin is wherein a kind of of polyvinyl alcohol, polyacrylic resin, polyvidone or wherein arbitrarily two kinds of weight ratio.
Polyacrylic resin can be EUDRAGIT NE 30 D EUDRAGIT NE 30D Eudragit E30D (Acrylic Acid Ethyl Ester-Methacrylic Acid Methyl Ester Copolymer), dimethylaminoethyl methacrylate-neutral methacrylic acid esters copolymer Eudragit E100, methacrylic acid-methyl acrylate copolymer Eudragit L100-55, neutral EUDRAGIT NE 30 D EUDRAGIT NE 30D Eudragit NE30D, methacrylic acid three ammoniums ethyl ester-polyacrylic resins such as acrylate copolymer Eudragit RL all has sale on market.
Used its degree of polymerization of polyvinyl alcohol Polyving Alcohol (PVA) is 500-1700, is specially PVAC polyvinylalcohol-0588, but the degree of polymerization such as hyoscine such as PVAC polyvinylalcohol-1788 grade is respectively 500,1700.
Used alcohols is ethanol, the glycerol a kind of or ethanol wherein and the mixture of any weight ratio of glycerol, and the amount that is added is the 1-12 weight portion, is advisable with the 4-12 weight portion, and the weight ratio of ethanol and glycerol is 1: 1～2.5 for well.
Said starch and derivant thereof are that corn soluble starch, Rhizoma Solani tuber osi soluble starch, carboxymethyl starch, carboxymethyl starch sodium, dextrin are wherein a kind of, the mixture of any weight ratio of two kinds or more than one, the amount that is added is the 1-15 weight portion, is good with the 2-8 weight portion again.
Said weight portion can be unit of weights such as gram, jin, kilogram, ton.
The preparation method of Capsules of the present invention is a raw material with vegetable polysaccharides Capsules feedstock composition, may further comprise the steps:
(1) gets raw material for standby by the weight portion of each component;
K-carrageenan 0.5-26 weight portion, cellulose derivative and/or resin 75-98 weight portion, alcohols 1-12 weight portion,
Said cellulose derivative is wherein a kind of of hypromellose, ethyl cellulose, hydroxypropyl cellulose, carboxymethyl cellulose or wherein arbitrarily two kinds of weight ratio;
Said resin is wherein a kind of of polyvinyl alcohol, polyacrylic resin, polyvidone or wherein arbitrarily two kinds of weight ratio; Above-mentioned polyvinyl alcohol is PVAC polyvinylalcohol-0588 or PVAC polyvinylalcohol-1788, and its degree of polymerization is respectively 500 and 1700; Above-mentioned polyacrylic resin is EUDRAGIT NE 30 D EUDRAGIT NE 30D Eudragit E30D, dimethylaminoethyl methacrylate-neutral methacrylic acid esters copolymer EudragitE100, methacrylic acid-methyl acrylate copolymer Eudragit L100-55, neutral EUDRAGIT NE 30 D EUDRAGIT NE 30D EudragitNE30D, methacrylic acid three ammoniums ethyl ester-acrylate copolymer Eudragit RL;
Said alcohols is ethanol, the glycerol a kind of or ethanol wherein and the mixture of any weight ratio of glycerol;
Do not contain potassium ion or calcium ion in the above-mentioned raw materials of the present invention.
(2) except that alcohols feedstock, the raw material that will get by each component places in the reaction vessel, 4 times-10 times water of the weight portion sum of the each component of adding except that alcohols feedstock under 65 ℃-85 ℃ temperature, makes material dissolution, form glue, in the material dissolution process, add alcohols feedstock.
(3) glue of Xing Chenging is incubated 1-24 hour under 30 ℃-60 ℃ temperature.
(4) through dipping in glue, oven dry (promptly dry), demoulding (promptly dialling shell), cutting, the synthetic product Capsules of cover.
When stirring, its mixing speed does not have great influence to the quality of product, and glue is non-foaming for well but it stirs speed.
Its preferred version is: also have starch and derivant 1-15 weight portion thereof in the raw material, said starch and derivant thereof are that corn soluble starch, Rhizoma Solani tuber osi soluble starch, carboxymethyl starch sodium, carboxymethyl starch, dextrin are wherein a kind of, wherein a kind of of the mixture of two or more any weight ratio, and its starch and derivant thereof add in the reactor with K-carrageenan, cellulose derivative and/or resin.The glue that forms is incubated 1-24 hour under 30-60 ℃ temperature, be good with 2-16 hour again.
Used raw material can be the commercially available K-carrageenan that does not contain potassium salt, is good with the K-carrageenan with following method preparation again.
Mixture with carrageenan is a raw material, the concentration that adds PH＞7～9 in the mixture of carrageenan is the ethanol water of 10%-60% percentage by volume, forms mixture, under 55 ℃-85 ℃ temperature backflow 0.5-2.5 hour, be placed to room temperature, filter the K-carrageenan.
In commercially available return tank (ZN type, medication chemistry container maker product) adds 1 kilogram of delicatessen food additive grade carrageenan mixture as raw material in, the concentration that adds PH=8.5 in the carrageenan mixture is the ethanol water of 35% percentage by volume, forms mixture.The amount of raw material carrageenan and the concentration of PH=8.5 are that the weight ratio of the ethanol water amount of 35% percentage by volume is 1: 2, under 80 ℃ temperature, refluxed 1.5 hours, be placed to 25 ℃ of room temperatures, behind filter paper filtering, with the concentration of PH=8.5 is the ethanol water washing 3 times of 35% percentage by volume, being dried to moisture in the calorstat that the washing back is used with commercially available laboratory under 70 ℃ temperature (DPH-240 type, the bright Medical Instruments in Beijing factory) is 11% percetage by weight.Through pressing 26 editions described infrared spectrometry test passes of American Pharmacopeia, its gel strength is 1200g/cm after tested
2, its kinematic viscosity is 90mm
2/ s (using the Ping Shi viscometer determining).
Dipping in method and the process conditions and the used equipment of operations such as glue, oven dry (drying), demoulding (dialling shell), cutting, fit, is that the person of ordinary skill in the field all knows.For example utilize mobile hot air dries (drying), room temperature remains on 30 ℃-35 ℃, and the thermal air current speed control got final product built in 1-17m/s in general 30-40 minute.Used reactor is reaction pot again, changes glue jar (Xinchang, Zhejiang modern pharmaceutical plant equipment factory product).
Can dip in glue, oven dry with the hard capsule glued membrane machine that Ninghai, Zhejiang Yongan machinery plant produces.With model is that the efficient capsule punching machine (county magistrate river, Xinchang, Zhejiang machinery plant) automatically of WP-645 cuts.Be that JN26MAB capsule automatic forming production line (Xinchang, Zhejiang morning twilight electromechanical research institute) is produced certainly with model.The Canadian production capsule manufacture line of import is good.
The excellent results of a kind of vegetable polysaccharides Capsules feedstock composition of the present invention and preparation method thereof just is:
1. the capsule that is come out as feedstock production by vegetable polysaccharides Capsules feedstock composition of the present invention not only has good stability, and is indeformable under the environment of high temperature or high humidity, and embrittlement not under the exsiccant environment of cold is convenient to permanent storage.Because the vegetable polysaccharides that uses is raw material, can not propagate foot and mouth disease and bovine spongiform encephalopathy etc., has avoided the pollution that may be caused by the animal proteinum protein.Under normal condition, the shelf-life was 18 months, and gastric solubleness is disintegrate fully in 10 minutes, and enteric is disintegrate fully in 60 minutes, met the regulation of the quality standard of the current edition Pharmacopoeia of the People's Republic of China.Can also be according to the requirement of medicine, the rate of release of control medicine also is suitable for containing the fill of aldehyde radical medicine and Chinese patent medicine oral solid formulation.
2. technology of the present invention can utilize original equipment to prepare capsule, small investment, and technology is simple.
The specific embodiment
Below with embodiment the preparation method of a kind of vegetable polysaccharides Capsules feedstock composition of the present invention and Capsules is further described; this will help the present invention and effect thereof are further understood; embodiment does not limit protection scope of the present invention, and its protection domain is decided by claim.
Embodiment 1
Used vegetable polysaccharides Capsules feedstock composition is 3 kilograms of K-carrageenans, 85 kilograms of hypromelloses, 4 kilograms of carboxymethyl starch sodium, 8 kilograms of glycerol in the present embodiment.
Its preparation method is:
(1) gets 3 kilograms of K-carrageenans, 85 kilograms of hypromelloses, 4 kilograms of carboxymethyl starch sodium, 8 kilograms of glycerol.
(2) with K-carrageenan, hypromellose, carboxymethyl starch sodium, place reactor (changing the glue jar), the water that adds 4 times of K-carrageenans, hypromellose, carboxymethyl starch sodium gross weight makes material dissolution form glue under 70 ℃ temperature, adds glycerol in the material dissolution process.
(3) glue of Xing Chenging is incubated 20 hours under 60 ℃ temperature, supports glue.
(4) during in 35 ℃, dip in glue, oven dry, demoulding, cutting, fit, check, lettering, packing, sterilization at glue temperature.
Disintegrate is complete in the Capsules that present embodiment is made, gastric solubleness 7 minutes, and the shelf-life was 18 months under normal operation.High temperature resistant, high humidity, cold resistant meet the quality standard of current edition Pharmacopoeia of the People's Republic of China defined fully.
Embodiment 2
Used process equipment and feedstock composition are substantially with embodiment 1, and only different is not have carboxymethyl starch sodium in the feedstock composition, and the Capsules of making is in gastric solubleness complete disintegrate in 10 minutes.
Embodiment 3
Used process equipment and feedstock composition are substantially with embodiment 1, and only different is 1 kilogram of K-carrageenan in the feedstock composition, corn soluble starch or 10 kilograms of Rhizoma Solani tuber osi soluble starches, 98 kilograms of hypromelloses, 6 kilograms of ethanol, 6 kilograms of glycerol.
Its preparation technology is: with K-carrageenan, corn soluble starch or Rhizoma Solani tuber osi soluble starch, hypromellose, in the placing glue jar, 8 times the water that adds K-carrageenan, corn soluble starch or Rhizoma Solani tuber osi soluble starch, hypromellose gross weight, under 65 ℃ of temperature, form glue, in the material dissolution process, add ethanol and glycerol, made Capsules in 12 hours in 30 ℃ of foster glue, disintegrate fully in the gastric solubleness 8 minutes.
Embodiment 4
Used process equipment and feedstock composition are substantially with embodiment 1, and only different is 2.3 kilograms of K-carrageenans, 80 kilograms of hydroxypropyl celluloses, and 1 kilogram of dextrin, the amount of ethanol and glycerol is 4 kilograms, the weight ratio of ethanol and glycerol is 1: 2.
Its preparation method is: in K-carrageenan, hydroxypropyl cellulose, placing of dextrin glue jar, 6 times the water that adds K-carrageenan, hydroxypropyl cellulose, dextrin gross weight, under 85 ℃ of temperature, form glue, the mixture that in the material dissolution process, adds ethanol and propanol, under 45 ℃ temperature, supported glue 8 hours, the Capsules gastric solubleness of making complete disintegrate in 9 minutes.
Embodiment 5
Used process equipment and feedstock composition are substantially with embodiment 1, and only different is 10 kilograms of K-carrageenans, 90 kilograms of hypromelloses, 8 kilograms of carboxymethyl starch sodium, 11 kilograms of glycerol.
Its preparation method is: in K-carrageenan, carboxylic third methylcellulose, placing of carboxymethyl starch sodium glue jar, 7 times the water that adds K-carrageenan, carboxylic third methylcellulose, carboxymethyl starch sodium gross weight, under 80 ℃ of temperature, form glue, in the material dissolution process, add glycerol, under 55 ℃ temperature, supported glue 24 hours, the Capsules gastric solubleness of making complete disintegrate in 9 minutes.
Embodiment 6
Used process equipment and feedstock composition are substantially with embodiment 5, and only different is to replace the Capsules complete disintegrate of gastric solubleness in 9 minutes that hypromellose is made for 90 kilograms with ethyl cellulose.
Embodiment 7
Used process equipment and feedstock composition are substantially with embodiment 5, and only different is the Capsules gastric solubleness complete disintegrate in 9.5 minutes made from 96 kilograms of hydroxypropyl celluloses.
Embodiment 8
Used process equipment and feedstock composition are substantially with embodiment 1, and only different is 2 kilograms of carrageenans, 500,85 kilograms of PVAC polyvinylalcohol-0588, the degree of polymerization, 10 kilograms of corn soluble starches, 6 kilograms of ethanol, 6 kilograms of glycerol.
Its preparation method is with K-carrageenan, PVAC polyvinylalcohol-0588, placing of corn soluble starch glue jar, the water that adds 6.5 times of K-carrageenans, PVAC polyvinylalcohol-0588, corn soluble starch gross weight, under 80 ℃ temperature, form glue, in the material dissolution process, add ethanol and glycerol, under 45 ℃ temperature, supported glue 16 hours, the Capsules gastric solubleness of making complete disintegrate in 8.5 minutes.
Embodiment 9
Used process equipment and feedstock composition be substantially with embodiment 1,1700,94 kilograms of only different is 0.5 kilogram of carrageenans, PVAC polyvinylalcohol-1788, the degree of polymerization, 10 kilograms of corn soluble starches, 8 kilograms of ethanol, 4 kilograms of glycerol.
Its preparation method is: in K-carrageenan, PVAC polyvinylalcohol-1788, the degree of polymerization 1700, placing of corn soluble starch glue jar, add K-carrageenan, PVAC polyvinylalcohol-1788, the water that corn soluble starch gross weight is 7.5 times, under 75 ℃ temperature, form glue, in the material dissolution process, add ethanol and glycerol, under 57 ℃ temperature, support glue 10 hours, make the complete disintegrate in 9.6 minutes of Capsules gastric solubleness.
Embodiment 10
Used process equipment and feedstock composition are substantially with embodiment 8, and only different is that adding PVAC polyvinylalcohol-0588, the degree of polymerization 500 are 80 kilograms of replacement PVA-1788, the Capsules gastric solubleness of making complete disintegrate in 8.0 minutes.
Embodiment 11
Used process equipment and feedstock composition are substantially with embodiment 8, and only different is 10 kilograms of corn soluble starch, carboxymethyl starch sodium, and the weight ratio of corn soluble starch and carboxymethyl starch sodium is 1: 1.5.
Embodiment 12
Used process equipment and feedstock composition are substantially with embodiment 8, only different is 3 kilograms of carrageenans, PVAC polyvinylalcohol-0588, the degree of polymerization 500 are 93 kilograms with the total amount of carboxymethyl cellulose, PVAC polyvinylalcohol-0588 is 1: 1 with the weight ratio of hypromellose, carboxymethyl starch sodium is 9 kilograms, 5 kilograms of ethanol, 6 kilograms of glycerol.
Its preparation method: with K-carrageenan, PVAC polyvinylalcohol-0588 and hypromellose, placing of carboxymethyl starch sodium glue jar, the water that adds 7.0 times of K-carrageenan, PVAC polyvinylalcohol-0588 and hypromellose, carboxymethyl starch sodium gross weights, under 75 ℃ temperature, form glue, in the material dissolution process, add ethanol and glycerol, under 60 ℃ temperature, supported glue 8 hours, the Capsules gastric solubleness of making complete disintegrate in 8.5 minutes.
Embodiment 13
Used process equipment and feedstock composition are substantially with embodiment 8, the gross weight of only different is 2.5 kilograms of K-carrageenans, PVAC polyvinylalcohol-1788, the degree of polymerization 1700 and hypromellose is that 90 kilograms, PVAC polyvinylalcohol-1788 are 1: 3 with the weight ratio of hypromellose, 8 kilograms of carboxymethyl starch sodium, 6 kilograms of glycerol.
Its preparation method: with K-carrageenan, PVAC polyvinylalcohol-1788 and hypromellose, placing of carboxymethyl starch sodium glue jar, 6.5 times the water that adds K-carrageenan, PVAC polyvinylalcohol-1788, hypromellose, carboxymethyl starch sodium gross weight, under 65 ℃ temperature, form glue, in the process of material dissolution, add glycerol, under 60 ℃ temperature, supported glue 10 hours, the Capsules gastric solubleness of making complete disintegrate in 8.5 minutes.
Embodiment 14
Used process equipment and feedstock composition are substantially with embodiment 1, and only different is 3.5 kilograms of K-carrageenans, 32 kilograms of hypromelloses, 53.5 kilograms of polyacrylic resins (EUDRAGIT NE 30 D EUDRAGIT NE 30D Eudragit E30D or methacrylic acid-methyl acrylate copolymer Eudragit L30D), 3 kilograms of carboxymethyl starch sodium, 8 kilograms of glycerol.
Its preparation method is: with the K-carrageenan, hypromellose, EUDRAGIT NE 30 D EUDRAGIT NE 30D E30D or methacrylic acid-methyl acrylate copolymer Eudragit L30D, in placing of the carboxymethyl starch sodium glue jar, add the K-carrageenan, hypromellose, EUDRAGIT NE 30 D EUDRAGIT NE 30D E30D or methacrylic acid-methyl acrylate copolymer Eudragit L30D, 7.0 times water of carboxymethyl starch sodium gross weight, under 75 ℃ temperature, form glue, in the material dissolution process, add glycerol, under 65 ℃ of temperature, supported glue 5 hours, the Capsules enteric of making complete disintegrate in 45 minutes.
Embodiment 15
Used process equipment and feedstock composition are substantially with embodiment 1, having only different is 0.5 kilogram of K-carrageenan, PVAC polyvinylalcohol-0588, the degree of polymerization 500,55 kilograms, 20 kilograms of polyacrylic resin EudragitL100 or Eudragit (100-55), 15 kilograms of corn soluble starches, glycerol and 10 kilograms of total ethanol weight, ethanol: the weight ratio of glycerol is 1: 1.
Its preparation method is: in K-carrageenan, PVAC polyvinylalcohol-0588, Eudragit L100 or Eudragit L100-55, placing of corn soluble starch glue jar, the water that adds 7.0 times of K-carrageenan, PVAC polyvinylalcohol-0588, Eudragit L100 or Eudragit L100-55, corn soluble starch gross weights, under 80 ℃ temperature, form glue, the mixture that adds ethanol and glycerol in the material dissolution process was in 80 ℃ of foster glue 3 hours.The Capsules enteric of making complete disintegrate in 30 minutes.
Embodiment 16
Used process equipment and feedstock composition be substantially with embodiment 1, and having only different is 5 kilograms of K-carrageenans, 50 kilograms of PVAC polyvinylalcohol-1788,33 kilograms of E30D, 6 kilograms of ethanol, 6 kilograms of glycerol.
Its technical process is fully with embodiment 15.Only do not add starch, enteric complete disintegrate in 45 minutes.
Embodiment 17
Used process equipment and feedstock composition are substantially with embodiment 16, and only different is 4 kilograms of K-carrageenans, PVAC polyvinylalcohol-0588,500,33 kilograms of the degree of polymerization, 62 kilograms of E30D polyacrylic resins, 4 kilograms of ethanol, 8 kilograms of glycerol.
Its preparation method is: in K-carrageenan, PVAC polyvinylalcohol-0588, placing of E30D polyacrylic resin glue jar, the water that adds 10 times of K-carrageenans, PVAC polyvinylalcohol-0588, E30D polyacrylic resin gross weight, under 81 ℃ temperature, form glue, in the material dissolution process, add ethanol and glycerol, in 85 ℃ of foster glue 2 hours.The Capsules of making is a slow releasing capsule.
Embodiment 18
Used process equipment and feedstock composition are substantially with embodiment 1, and only different is 22 kilograms of K-carrageenans, 90 kilograms of hypromelloses, 15 kilograms of carboxymethyl starch sodium, 12 kilograms of glycerol.
Its preparation method is: 7 times of water that add K-carrageenan, hypromellose, carboxymethyl starch sodium gross weight, under 80 ℃ temperature, form glue, in the material dissolution process, add glycerol, under 55 ℃ temperature, supported glue 24 hours, make plant hollow capsule, gastric solubleness loose 10 minutes.
Embodiment 19
Used process equipment and feedstock composition are substantially with embodiment 18, and only different is 20 kilograms of K-carrageenans, 93 kilograms of hypromelloses.
Embodiment 20
Used process equipment and feedstock composition are substantially with embodiment 19, and only different is 26 kilograms of K-carrageenans.
Claims (15)
1, a kind of vegetable polysaccharides Capsules feedstock composition is characterized in that, comprises K-carrageenan 0.5-26 weight portion, cellulose derivative and/or resin 75-98 weight portion, alcohols 1-12 weight portion;
Said cellulose derivative is wherein a kind of of hypromellose, ethyl cellulose, hydroxypropyl cellulose, carboxymethyl cellulose or wherein arbitrarily two kinds of weight ratio;
Said resin is wherein a kind of of polyvinyl alcohol, polyacrylic resin, polyvidone or wherein arbitrarily two kinds of weight ratio; Above-mentioned polyvinyl alcohol is PVAC polyvinylalcohol-0588 or PVAC polyvinylalcohol-1788, and its degree of polymerization is respectively 500 and 1700; Above-mentioned polyacrylic resin is EUDRAGIT NE 30 D EUDRAGIT NE 30D Eudragit E30D, dimethylaminoethyl methacrylate-neutral methacrylic acid esters copolymer Eudragit E100, methacrylic acid-methyl acrylate copolymer Eudragit L100-55, neutral EUDRAGIT NE 30 D EUDRAGIT NE 30D Eudragit NE30D, methacrylic acid three ammoniums ethyl ester-acrylate copolymer Eudragit RL;
Said alcohols is ethanol, the glycerol a kind of or ethanol wherein and the mixture of any weight ratio of glycerol;
Said composition does not conform to potassium ion or calcium ion.
2, according to a kind of vegetable polysaccharides Capsules feedstock composition of claim 1, it is characterized in that, also comprise starch or derivatives thereof 1-15 weight portion, said starch and derivant thereof are that corn soluble starch, Rhizoma Solani tuber osi soluble starch, carboxymethyl starch sodium, carboxymethyl starch, dextrin are wherein a kind of, wherein a kind of of the mixture of two or more any weight ratio.
3, according to a kind of vegetable polysaccharides Capsules feedstock composition of claim 1, it is characterized in that the amount of cellulose derivative and/or resin is the 90-96 weight portion.
4, according to a kind of vegetable polysaccharides Capsules feedstock composition of claim 1, it is characterized in that the amount of the mixture of polyvinyl alcohol and cellulose derivative is the 75-98 weight portion.
5, according to a kind of vegetable polysaccharides Capsules feedstock composition of claim 4, it is characterized in that the amount of the mixture of polyvinyl alcohol and cellulose derivative is the 90-96 weight portion.
6, according to claim 4,5 one of them a kind of vegetable polysaccharides Capsules feedstock compositions, it is characterized in that, starch and derivant thereof are the 1-15 weight portion, and said starch and derivant thereof are that corn soluble starch, Rhizoma Solani tuber osi soluble starch, carboxymethyl starch sodium, carboxymethyl starch, dextrin are wherein a kind of, wherein a kind of of the mixture of two or more any weight ratio.
7, according to claim 4,5 one of them a kind of vegetable polysaccharides Capsules feedstock compositions, it is characterized in that the weight ratio of polyvinyl alcohol and cellulose derivative is 1: 1～3.
8, according to a kind of vegetable polysaccharides Capsules feedstock composition of claim 1, it is characterized in that the K-carrageenan is the 2-10 weight portion.
9, a kind of vegetable polysaccharides Capsules feedstock composition according to Claim 8 is characterized in that, the K-carrageenan is 2.3-＜4.2 weight portions.
10, according to a kind of vegetable polysaccharides Capsules feedstock composition of claim 1, it is characterized in that the amount of said alcohols is the 4-12 weight portion.
11, according to a kind of vegetable polysaccharides Capsules feedstock composition of claim 1, it is characterized in that the weight ratio of ethanol and glycerol is 1: 1～2.5.
12, according to a kind of vegetable polysaccharides Capsules feedstock composition of claim 2, it is characterized in that starch and derivant thereof are the 2-8 weight portion.
13, a kind of preparation method of Capsules is characterized in that, is raw material with vegetable polysaccharides Capsules feedstock composition, may further comprise the steps:
(1) gets raw material for standby by the weight portion of each component;
K-carrageenan 0.5-26 weight portion, cellulose derivative and/or resin 75-98 weight portion, alcohols 1-12 weight portion,
Said cellulose derivative is wherein a kind of of hypromellose, ethyl cellulose, hydroxypropyl cellulose, carboxymethyl cellulose or wherein arbitrarily two kinds of weight ratio;
Said resin is wherein a kind of of polyvinyl alcohol, polyacrylic resin, polyvidone or wherein arbitrarily two kinds of weight ratio; Above-mentioned polyvinyl alcohol is a PVAC polyvinylalcohol-0588, PVAC polyvinylalcohol-1788, and its degree of polymerization is respectively 500 and 1700; Above-mentioned polyacrylic resin is EUDRAGIT NE 30 D EUDRAGIT NE 30D Eudragit E30D, dimethylaminoethyl methacrylate-neutral methacrylic acid esters copolymer Eudragit E100, methacrylic acid-methyl acrylate copolymer Eudragit L100-55, neutral EUDRAGIT NE 30 D EUDRAGIT NE 30D EudragitNE30D, methacrylic acid three ammoniums ethyl ester-acrylate copolymer Eudragit RL;
Said alcohols is ethanol, the glycerol a kind of and ethanol wherein and the mixture of any weight ratio of glycerol;
Do not contain potassium ion or calcium ion in the raw material;
(2) except that alcohols feedstock, the raw material that to be got by the each component weight portion, place 4 times of-10 times of water that add the weight portion sum of the each component except that alcohols feedstock in the reaction vessel, temperature in 65-85 ℃, under agitation, make material dissolution, form glue, in the material dissolution process, add alcohols feedstock;
(3) formed glue is incubated 1-24 hour under 30-60 ℃ temperature;
(4) through dipping in glue, oven dry, demoulding, cutting, the synthetic product Capsules of cover.
14, according to the preparation method of a kind of Capsules of claim 13, it is characterized in that glue is incubated 2-16 hour under 30-60 ℃ temperature.
15, according to the preparation method of a kind of Capsules of claim 13, it is characterized in that, also have starch and derivant 1-15 weight portion thereof in the raw material, said starch and derivant thereof are that corn soluble starch, Rhizoma Solani tuber osi soluble starch, carboxymethyl starch sodium, carboxymethyl starch, dextrin are wherein a kind of, wherein a kind of of the mixture of two or more any weight ratio, and its starch and derivant thereof add in the reactor with K-carrageenan, cellulose derivative and/or resin.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510079888 CN1276779C (en) | 2005-07-01 | 2005-07-01 | Hollow capsule material composition of plant polysaccharide and production of hollow capsule |
| PCT/CN2006/001480 WO2007003113A1 (en) | 2005-07-01 | 2006-06-28 | A composition of raw materials for a plant polyose-containing hollow capsule and the properation method of such capsure |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200510079888 CN1276779C (en) | 2005-07-01 | 2005-07-01 | Hollow capsule material composition of plant polysaccharide and production of hollow capsule |
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| CN1276779C true CN1276779C (en) | 2006-09-27 |
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| CN 200510079888 Active CN1276779C (en) | 2005-07-01 | 2005-07-01 | Hollow capsule material composition of plant polysaccharide and production of hollow capsule |
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| CN (1) | CN1276779C (en) |
| WO (1) | WO2007003113A1 (en) |
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| EP2179728A4 (en) * | 2007-08-10 | 2013-01-23 | Shanghai Huiyuan Vegetal Capsule Co Ltd | Non-gelatin shell material of hard capsule and process for preparing thereof |
| EP2223685A4 (en) * | 2007-11-13 | 2013-08-21 | Shanghai Huiyuan Vegetal Capsule Co Ltd | Non-gelatin enteric hard capsule shell and preparation method thereof |
| CN101596146B (en) * | 2008-06-06 | 2013-03-27 | 中国科学院海洋研究所 | Method for controlling temperature in the production process of seaweed polysaccharide plant empty capsules |
| CN102429889A (en) * | 2011-11-30 | 2012-05-02 | 无锡福祈制药有限公司 | Large ring lactone type medicament capsule and preparation method thereof |
| CN102499985B (en) * | 2011-12-15 | 2013-04-17 | 山西吉呈生物技术有限公司 | Hard-shell capsule based on cellulose |
| CN102579391A (en) * | 2012-03-05 | 2012-07-18 | 北京皇岛海洋生物科技有限公司 | Gastric soluble compound seaweed polysaccharide film coating premix and liquid preparation method adopting same |
| US11312878B2 (en) | 2012-07-23 | 2022-04-26 | Lotte Fine Chemical Co., Ltd. | Aqueous composition for preparing hard capsule, preparation method therefor, hard capsule, and method for recycling hard capsule scraps |
| CN102895215A (en) * | 2012-10-18 | 2013-01-30 | 广西南宁汇润生物科技有限公司 | Cellulose and red alga polysaccharide plant empty capsule and raw material composition and preparation method thereof |
| KR102085330B1 (en) | 2012-12-05 | 2020-03-05 | 롯데정밀화학 주식회사 | Hard capsule having improved thickness uniformity |
| CN103768608B (en) * | 2014-02-05 | 2016-12-14 | 石狮市新明食品科技开发有限公司 | A kind of plant capsule compositions of Sargassum colloid |
| CN103893771B (en) * | 2014-04-21 | 2015-08-26 | 湖南尔康制药股份有限公司 | A kind of film-forming composition for the production of starch material soft capsule and preparation method thereof |
| CN104758271A (en) * | 2015-03-16 | 2015-07-08 | 中华生物科技有限公司 | Plant vacant capsule compounded from cellulose gum and red alga KAPPA gum and preparation method thereof |
| CN105434394B (en) * | 2015-12-16 | 2019-01-25 | 刘松林 | A kind of polyvinyl alcohol Capsules |
| CN107674354B (en) * | 2017-10-18 | 2020-11-17 | 无锡鼎加弘思饮品科技有限公司 | Soluble coffee capsule cup body, preparation method thereof and coffee capsule |
| CN107890113A (en) * | 2017-12-21 | 2018-04-10 | 瑞昌市渝瑞实业有限公司 | Chinese yam hard capsules production system and production method |
| CN109364039A (en) * | 2018-09-21 | 2019-02-22 | 浙江中同科技有限公司 | A kind of starch hollow capsule and preparation method thereof |
| CN109966501A (en) * | 2019-05-09 | 2019-07-05 | 徐燕滨 | Sodium carboxymethyl starch is preparing application and hard capsule in plant polyose hard capsule |
| CN114306272A (en) * | 2019-06-12 | 2022-04-12 | 江苏艾兰得营养品有限公司 | Plant soft capsule and preparation method and application thereof |
| CN112826115B (en) * | 2020-10-10 | 2022-04-08 | 广州玖洲胶囊生物科技有限公司 | Preparation method of hollow capsule capable of achieving targeted release in intestinal tract |
| CN113876739B (en) * | 2021-11-15 | 2023-04-25 | 新昌中国计量大学企业创新研究院有限公司 | Plant hollow capsule and preparation method thereof |
| CN115282125B (en) * | 2022-06-27 | 2023-07-21 | 江苏辰星药业股份有限公司 | Antibacterial hollow capsule and preparation method thereof |
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| JPH07196478A (en) * | 1993-12-30 | 1995-08-01 | Hajime Sugii | Soft capsule for highly safe food and medicine |
| CN1292261A (en) * | 1999-09-28 | 2001-04-25 | 上海大众凌伟生化股份有限公司 | Plant hard capsule and its production process |
| US6949256B2 (en) * | 2002-01-18 | 2005-09-27 | Banner Pharmacaps, Inc. | Non-gelatin capsule shell formulation |
| CN1606978A (en) * | 2003-10-15 | 2005-04-20 | 浙江省新昌县药联胶丸有限公司 | Hollow capsule of natural plant gum and its preparing process |
| CN100393296C (en) * | 2004-12-09 | 2008-06-11 | 浙江工业大学 | Formula of making hollow capsule and its preparation method |
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2005
- 2005-07-01 CN CN 200510079888 patent/CN1276779C/en active Active
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- 2006-06-28 WO PCT/CN2006/001480 patent/WO2007003113A1/en active Application Filing
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| WO2007003113A1 (en) | 2007-01-11 |
| CN1745745A (en) | 2006-03-15 |
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