CN100577136C - 水凝胶、水凝胶的制备方法及其用途 - Google Patents
水凝胶、水凝胶的制备方法及其用途 Download PDFInfo
- Publication number
- CN100577136C CN100577136C CN200610171440A CN200610171440A CN100577136C CN 100577136 C CN100577136 C CN 100577136C CN 200610171440 A CN200610171440 A CN 200610171440A CN 200610171440 A CN200610171440 A CN 200610171440A CN 100577136 C CN100577136 C CN 100577136C
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- CN
- China
- Prior art keywords
- ascorbic acid
- hydrogel
- acid
- aluminium
- gel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 238000004519 manufacturing process Methods 0.000 title description 11
- -1 aluminum compound Chemical class 0.000 claims abstract description 63
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 51
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 44
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 44
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 23
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims abstract description 22
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims abstract description 22
- 229920000642 polymer Polymers 0.000 claims abstract description 21
- 229920002125 Sokalan® Polymers 0.000 claims abstract description 20
- 239000004584 polyacrylic acid Substances 0.000 claims abstract description 18
- 239000008213 purified water Substances 0.000 claims abstract description 14
- 239000000017 hydrogel Substances 0.000 claims description 99
- 239000000499 gel Substances 0.000 claims description 42
- 239000000203 mixture Substances 0.000 claims description 20
- 238000002360 preparation method Methods 0.000 claims description 19
- 150000001399 aluminium compounds Chemical class 0.000 claims description 18
- 230000007935 neutral effect Effects 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 13
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 11
- OCYUQKSNQVZPED-UHFFFAOYSA-L aluminum;magnesium;dihydroxide Chemical compound [OH-].[OH-].[Mg+2].[Al+3] OCYUQKSNQVZPED-UHFFFAOYSA-L 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 9
- 238000010998 test method Methods 0.000 claims description 9
- 239000002537 cosmetic Substances 0.000 claims description 8
- 150000002148 esters Chemical class 0.000 claims description 7
- 239000011777 magnesium Substances 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- 150000005846 sugar alcohols Polymers 0.000 claims description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 6
- HTAWSOSQCJAPJB-UHFFFAOYSA-H [Al+3].NCC(=O)[O-].O[Al+]O.NCC(=O)[O-].NCC(=O)[O-].NCC(=O)[O-] Chemical compound [Al+3].NCC(=O)[O-].O[Al+]O.NCC(=O)[O-].NCC(=O)[O-].NCC(=O)[O-] HTAWSOSQCJAPJB-UHFFFAOYSA-H 0.000 claims description 6
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 6
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 5
- PCRDIRUKXOTDNN-UHFFFAOYSA-K aluminum;sodium;carbonate;hydroxide Chemical compound [OH-].[Na+].[Al+3].[O-]C([O-])=O PCRDIRUKXOTDNN-UHFFFAOYSA-K 0.000 claims description 4
- 150000003863 ammonium salts Chemical class 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- GRLPQNLYRHEGIJ-UHFFFAOYSA-J potassium aluminium sulfate Chemical compound [Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRLPQNLYRHEGIJ-UHFFFAOYSA-J 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- 239000010409 thin film Substances 0.000 claims description 3
- MLSJBGYKDYSOAE-DCWMUDTNSA-N L-Ascorbic acid-2-glucoside Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O[C@@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)=C1O MLSJBGYKDYSOAE-DCWMUDTNSA-N 0.000 claims description 2
- XDBMXUKHMOFBPJ-ZAFYKAAXSA-N L-ascorbic acid 2-sulfate Chemical compound OC[C@H](O)[C@H]1OC(=O)C(OS(O)(=O)=O)=C1O XDBMXUKHMOFBPJ-ZAFYKAAXSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 229920000388 Polyphosphate Polymers 0.000 claims description 2
- 229940072065 ascorbic acid 2-sulfate Drugs 0.000 claims description 2
- 125000002768 hydroxyalkyl group Chemical group 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000001205 polyphosphate Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 12
- 229910052782 aluminium Inorganic materials 0.000 abstract description 11
- TYQCGQRIZGCHNB-JLAZNSOCSA-N l-ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(O)=C(O)C1=O TYQCGQRIZGCHNB-JLAZNSOCSA-N 0.000 description 37
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 29
- 229920001577 copolymer Polymers 0.000 description 29
- 239000000284 extract Substances 0.000 description 26
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 16
- 239000003814 drug Substances 0.000 description 16
- 229940047670 sodium acrylate Drugs 0.000 description 16
- 239000000126 substance Substances 0.000 description 16
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 description 15
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 15
- 239000008279 sol Substances 0.000 description 15
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 14
- LVTYICIALWPMFW-UHFFFAOYSA-N diisopropanolamine Chemical compound CC(O)CNCC(C)O LVTYICIALWPMFW-UHFFFAOYSA-N 0.000 description 14
- 229940043276 diisopropanolamine Drugs 0.000 description 14
- 239000011505 plaster Substances 0.000 description 14
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 13
- 239000004744 fabric Substances 0.000 description 13
- 239000002994 raw material Substances 0.000 description 13
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 12
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 12
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 12
- 239000003921 oil Substances 0.000 description 12
- 235000019198 oils Nutrition 0.000 description 12
- 229960002920 sorbitol Drugs 0.000 description 12
- 239000003795 chemical substances by application Substances 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 10
- 229960005150 glycerol Drugs 0.000 description 10
- 235000013599 spices Nutrition 0.000 description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- 239000006185 dispersion Substances 0.000 description 9
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 8
- 239000002253 acid Substances 0.000 description 8
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 8
- 229910021529 ammonia Inorganic materials 0.000 description 8
- 235000014113 dietary fatty acids Nutrition 0.000 description 8
- 239000000194 fatty acid Substances 0.000 description 8
- 229930195729 fatty acid Natural products 0.000 description 8
- 230000005070 ripening Effects 0.000 description 8
- 239000000600 sorbitol Substances 0.000 description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 7
- 235000003140 Panax quinquefolius Nutrition 0.000 description 7
- 240000005373 Panax quinquefolius Species 0.000 description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 235000019437 butane-1,3-diol Nutrition 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 230000001404 mediated effect Effects 0.000 description 7
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 7
- 229960004889 salicylic acid Drugs 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 239000003431 cross linking reagent Substances 0.000 description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000004137 magnesium phosphate Substances 0.000 description 6
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 6
- 229960002261 magnesium phosphate Drugs 0.000 description 6
- 229940091250 magnesium supplement Drugs 0.000 description 6
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 6
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- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 6
- MGSRCZKZVOBKFT-UHFFFAOYSA-N thymol Chemical compound CC(C)C1=CC=C(C)C=C1O MGSRCZKZVOBKFT-UHFFFAOYSA-N 0.000 description 6
- 108010010803 Gelatin Proteins 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0212—Face masks
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/365—Lactones
- A61K31/375—Ascorbic acid, i.e. vitamin C; Salts thereof
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K31/66—Phosphorus compounds
- A61K31/665—Phosphorus compounds having oxygen as a ring hetero atom, e.g. fosfomycin
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- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/06—Aluminium, calcium or magnesium; Compounds thereof, e.g. clay
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/32—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. carbomers, poly(meth)acrylates, or polyvinyl pyrrolidone
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- A—HUMAN NECESSITIES
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Abstract
本发明涉及一种基本包含至少两种选自聚丙烯酸、聚丙烯酸钠和部分中和的聚丙烯酸酯中的聚合物和水的水凝胶,其中所述聚合物通过包含铝化合物被交联,并且当所述水凝胶用纯化水稀释100倍时pH为6.5-8.5。提供了一种具备下述优点的水凝胶:能够稳定保持抗坏血酸或其衍生物,具有高凝胶强度,显示出与被粘附物的良好粘合,和不引起液体脱水收缩。
Description
本发明是专利申请No.03814058.6的分案申请,该专利申请的申请日是2003年6月18日,发明创造名称是“水凝胶、水凝胶的制备方法及其用途”。
相关申请的交叉参考
本申请是一项依照35U.S.C.§111(a)递交的申请,依照35U.S.C.§119(e)(1)要求享有临时申请60/423,375的申请日的权益,而所述临时申请是依照35U.S.C.§111(b)于2002年11月4日递交的。
技术领域
本发明涉及一种包含抗坏血酸或其衍生物的水凝胶、该水凝胶的制备方法和用途,其中所述水凝胶能够稳定地保持抗坏血酸或其衍生物,能够用于外用医疗制剂(例如模制泥敷剂、胶带剂或硬膏剂)、化妆品如化妆膏和伤口保护剂,能够显示高的自成型保持能力并易于生产。
背景技术
众所周知,抗坏血酸或其衍生物参与胶原的生物合成并尤其具有保持皮肤处于稳定新鲜状态的功能,防止产生导致斑点和雀斑的黑色素沉着,保持美丽的皮肤。但是,当抗坏血酸或其衍生物被形成进入用于皮肤的洗剂、面霜等时,所述制剂不能以恒定量涂覆以至不能提供均匀效果或由于与衣服接触被除去以至不能提供满意的效果。
为了解决这些问题,已知的一种方法是将抗坏血酸或其衍生物混入具有形状保持能力的水凝胶中并将该水凝胶施加到皮肤上。用于硬膏剂或冷隔离体(cold insulator)的水凝胶通常通过下述方式组成:使用天然水溶性聚合物如黄蓍胶、阿拉伯树胶、爱兰苔胶、Duran胶、藻酸钠、甘露聚糖和明胶,或合成聚合物如聚丙烯酸、聚甲基丙烯酸酯、聚乙烯醇和聚丙烯酰胺作为基体,并将其与湿润剂(例如多元醇)、水等混合。但是,天然水溶性聚合物是特别由天然产物获得的,因此,除非这些聚合物被提纯到较高水平,否则质量上不稳定,引起例如因混入成分污染或因杂质劣化的现象。
例如,日本未审定专利公开No.2001-64175(JP-A-2001-64175)公开了一种通过使用选自硅铝酸镁、干燥的氢氧化铝凝胶和氯化铝的两种化合物制备包含抗坏血酸或其衍生物的水凝胶的方法。但是,该方法不能充分维持凝胶的形状保持力。尤其在夏季水凝胶暴露于高温状态下,所述水凝胶出现下垂并且,有时引起所谓的“击穿”。因此,仍然存在有待解决的问题。
发明公开
本发明是在上述这些环境下完成的,其目的在于提供一种水凝胶,这种水凝胶能够稳定地保持抗坏血酸或其衍生物,具有高凝胶强度,显示良好的与被粘物的粘合,不引起液体脱水收缩,具有简单组成以便于制备,凝胶的制备迅速并能够以工业化方法生产。
为了解决上述问题,本发明人进行了广泛的实验研究,发现符合下述条件的水凝胶能够稳定保持抗坏血酸或其衍生物并显示优异的凝胶性能:该水凝胶基本包含至少两种选自聚丙烯酸、聚丙烯酸钠和部分中和的聚丙烯酸酯的聚合物,其中的聚合物通过交联剂、特别是铝化合物交联,并且当该水凝胶用纯化水稀释100倍时pH为6.5-8.5。在此发现的基础上完成了本发明。本发明提供下述(1)-(13)项描述的水凝胶、水凝胶生产方法及水凝胶的用途。
(1)一种包含凝胶、水和抗坏血酸或其衍生物的水凝胶,其中所述凝胶包含至少两种选自聚丙烯酸、聚丙烯酸钠和部分中和的用铝化合物交联的聚丙烯酸酯中的聚合物,并且当该水凝胶用纯化水稀释100倍时pH为6.5-8.5。
(2)如上述第(1)项所述的水凝胶,其中pH为7.0-8.0。
(3)如上述第(1)或(2)项所述的水凝胶,其中铝化合物是氢氧化镁-氢氧化铝共沉淀物。
(4)如上述第(1)-(3)中任一项所述的水凝胶,其中铝化合物的含量为按每100质量份水凝胶计0.01-10质量份。
(5)如上述第(1)-(4)中任一项所述的水凝胶,其中抗坏血酸或其衍生物的含量为按每100质量份水凝胶计0.01-10质量份。
(6)如上述第(1)-(5)中任一项所述的水凝胶,其中抗坏血酸衍生物是抗坏血酸-2-磷酸酯或其盐。
(7)如上述第(1)-(6)中任一项所述的水凝胶,其中水凝胶包含多元醇。
(8)如上述第(1)-(7)中任一项所述的水凝胶,其中当该水凝胶形成厚度0.5mm的薄膜并在25℃和相对湿度60%下暴露24小时后依照JIS Z0237粘着性测试方法(Tack Test Method)在其表面测试粘着性时,倾斜角为30°的球式粘着值(ball tack value)为10或更高。
(9)一种制备水凝胶的方法,包括制备含有至少两种选自聚丙烯酸、聚丙烯酸钠和部分中和的聚丙烯酸酯的聚合物、铝化合物、水和抗坏血酸或其衍生物的混合物,在25-65℃下加热该混合物。
(10)如上述第(9)项所述的制备水凝胶的方法,其中当所述水凝胶用纯化水稀释100倍时pH被调整为6.5-8.5。
(11)如上述第(10)项所述的制备水凝胶的方法,其中pH被调整为7.0-8.0。
(12)一种包含上述第(1)-(8)中任一项所述的水凝胶的化妆材料。
(13)一种包含上述第(1)-(8)中任一项所述的水凝胶的外用制剂。
实施本发明的最佳方式
下面将详细描述本发明
本发明水凝胶包含凝胶、水和抗坏血酸或其衍生物,其中所述凝胶包含至少两种选自聚丙烯酸、聚丙烯酸钠和部分中和的用铝化合物交联的聚丙烯酸酯中的聚合物,并且当该水凝胶用纯化水稀释100倍时pH为6.5-8.5。
本发明水凝胶能够稳定保持抗坏血酸或其衍生物并显示优异的凝胶性能。该水凝胶不具有流动性,具有强弹性并且即使用手指按压也不容易塌陷。依靠这些优异性能,本发明水凝胶可用于各种用途,例如医疗产品如硬膏剂(例如经皮吸收制剂、经粘膜吸收制剂)、化妆品和药用化妆品如化妆膏、防晒化妆品和粉刺化妆品。
抗坏血酸或其衍生物在本发明水凝胶中的使用量为基于100质量份水凝胶计的0.01-10质量份,优选0.5-5.0质量份。
抗坏血酸衍生物或其盐实际上是酶促或非酶促体内分解并释放抗坏血酸的抗坏血酸衍生物或其盐。具有所述性能的抗坏血酸衍生物或其盐的实例包括抗坏血酸-2-磷酸酯、抗坏血酸-2-焦磷酸酯、抗坏血酸-2-三磷酸酯、抗坏血酸-2-多磷酸酯、抗坏血酸-2,3-二磷酸酯、抗坏血酸-2,6-二磷酸酯、抗坏血酸-2-硫酸酯、抗坏血酸-6-棕榈酸酯、抗坏血酸-2,6-棕榈酸酯、抗坏血酸-2-葡糖苷、抗坏血酸-2-O-葡糖苷-6-棕榈酸酯、抗坏血酸-5,6-亚苄基、抗坏血酸-5,6-亚丙基和它们的金属盐、铵盐和烷基-或羟烷基取代的铵盐。
在这些抗坏血酸衍生物中,从效果和效力着眼,优选的化合物是抗坏血酸-2-磷酸酯和其盐,例如抗坏血酸-2-磷酸酯的镁盐和抗坏血酸-2-磷酸酯的钠盐。与已知的其它抗坏血酸衍生物相比,抗坏血酸-2-磷酸酯的活体吸收率较高,并且还显示出高的抗坏血酸体内释放率。这些盐可通过例如在日本未审定专利公开No.44-31237(JP-A-44-31237)描述的方法制备,或可以使用商业可得产品。
用作基体的水溶性聚合物聚丙烯酸、聚丙烯酸钠和部分中和的聚丙烯酸酯对皮肤刺激较低并具有高粘附性。在这些聚合物中,部分中和的聚丙烯酸酯包括其中一部分聚丙烯酸被碱中和的那些聚合物。碱的实例可包括碱金属盐如氢氧化钠、氢氧化钾,氨,氨水,伯、仲和叔烷基胺如三乙醇胺、二甲胺、二乙胺、三甲胺、三乙胺、三异丙醇胺和聚乙醇胺。部分中和的聚丙烯酸酯可通过部分中和聚丙烯酸酯或通过先部分中和丙烯酸单体原料然后聚合单体制备。在部分中和的聚丙烯酸酯中,丙烯酸成分与丙烯酸盐成分的摩尔比可优选为80∶20-20∶80,更优选为65∶35-35∶65。如果摩尔比超出此范围,凝胶(与铝离子的键接,即交联反应)率存在严重下降的趋势。部分中和聚丙烯酸酯的典型实例可包括丙烯酸钠/丙烯酸共聚物、丙烯酸钾/丙烯酸共聚物、丙烯酸铵/丙烯酸共聚物等,但本发明并不限于这些共聚物。在本发明水凝胶中,通过使用至少两种选自聚丙烯酸、聚丙烯酸钠和部分中和聚丙烯酸酯的聚合物可容易地进行凝胶化。其中的机理还不能清楚地了解,但是认为,在这些聚合物的游离羧基和羧酸盐之间进行钠盐的盐交换期间,由于铝离子的插入进行离子交联。
为了维持凝胶的形状保持性,作为交联剂加入的铝化合物的含量为按每100质量份水凝胶计0.01-10质量份,优选0.5-5.0质量份。如果添加量低于0.01质量份,交联进行得不充分以至凝胶强度差,并且获得的水凝胶可能在形状保持力方面严重劣化;反之,如果超过10质量份,凝胶硬化缺乏柔性并且可能难于形成形状。通过改变交联剂的用量,凝胶的弹力或柔性可得到自由控制并且与皮肤的适应性(附着)可得到改变。
铝化合物的实例包括氯化铝、硫酸铝钾、硫酸铝铵、硝酸铝、硫酸铝、EDTA-铝、氢氧化铝-碳酸氢钠的共沉淀物(例如,由Kyowa ChemicalIndustry Co.,Ltd.生产的“Kumulite”)、合成硅酸铝、硬脂酸铝、尿囊素铝(Aluminum allantoinate)、合成水滑石(例如由Kyowa ChemicalIndustry Co.,Ltd.生产的“Alcamac”,“Alcamizer”和“KYOWORD”)、氢氧化镁-氢氧化铝共沉淀物(例如由Kyowa Chemical Industry Co.,Ltd.生产的“Sanalmin”)、氢氧化铝(例如,由Kyowa Chemical Industry Co.,Ltd.生产的“干燥的氢氧化铝凝胶S-100”)、乙酸铝、氨基乙酸二羟基铝(例如,由Kyowa Chemical Industry Co.,Ltd.生产的“Glycinal”)、高岭土、硅铝酸镁(例如,由Fuji chemical Indusry Co.,Ltd.生产的“Neusilin”)和氨基硅酸镁。所述铝化合物可以是水溶性或微溶的。其中优选氢氧化铝镁,因为凝胶化能迅速进行并能够获得均匀的具有优异形状保持性的凝胶。这些铝化合物可以单独使用或以两种或多种组合的形式使用。
在本发明水凝胶中,还可以加入除铝化合物之外的交联剂,其实例包括钙、锡、铁、镁、锰、锌、钡等的无机酸盐(例如,氯化钙、氯化镁、铁明矾、硫酸铁、硫酸镁、EDTA-钙、EDTA-镁、氯化亚锡、碳酸钙、磷酸钙、磷酸氢镁、碳酸镁、硫酸钡、硅酸镁、硬脂酸镁和柠檬酸镁),氢氧化物(例如氢氧化钙、氢氧化钡、氢氧化镁(例如由Kyowa ChemicalIndustry Co.,Ltd.生产的“KISUMA”)、氢氧化铁和氢氧化亚锡),氧化物(例如氧化镁(例如Kyowa Chemical Industry Co.,Ltd.生产的“KYOWAMAG”、“MAGSALAT”),和甲醛、乙二醇缩水甘油醚、甘油缩水甘油醚、聚乙二醇缩水甘油醚、丙二醇缩水甘油醚和聚丙二醇缩水甘油醚的环氧化合物。这些交联剂可以单独使用或以两种或多种组合的方式使用。
为了提高水凝胶的保湿能力或增强抗坏血酸或其衍生物的效果,本发明水凝胶中优选添加多元醇。所述多元醇的实例包括乙二醇、丙二醇、1,3-丁二醇、二甘醇、三甘醇、1,4-丁二醇(二元醇)、甘油、三氧代异丁烷(三元醇)、赤藻糖醇、季戊四醇(四元醇)、木糖醇、戊五醇(五元醇)、异半乳糖醇(allodulcitol)、山梨糖醇、液体山梨糖醇和甘露醇(六元醇),但是本发明并不仅限于此。
当用纯化水稀释100倍(质量)时,本发明水凝胶的pH为6.5-8.5,优选7.0-8.0。如果pH超过该范围,抗坏血酸或其衍生物的稳定性严重劣化并且不能获得希望的效果。对测量pH的方法没有特殊限制,可以使用普通pH仪。
对pH进行调节不仅为了确保抗坏血酸或其衍生物的稳定性,而且用于控制交联率。可以用于生产本发明水凝胶的pH调节剂的实例包括碱如碱金属的氢氧化物,碱土金属的氢氧化物,伯、仲或叔烷基胺、和伯、仲或叔链烷醇胺,例如氢氧化钠、氢氧化钾、氢氧化钙、氢氧化镁、氨,氨水、三乙醇胺、二甲胺、二乙胺、三甲胺、三乙胺、三异丙醇胺、磷酸三钠、磷酸氢二钠、磷酸氢二钾、一乙醇胺、二乙醇胺、二异丙醇胺和聚乙醇胺。此外,可以使用对金属离子具有螯合或配位能力的有机酸、有机酸盐和有机碱,例如柠檬酸、酒石酸、乳酸、羟基乙酸、盐酸、硝酸、苹果酸、磷酸、水杨酸、富马酸、甲磺酸、马来酸、乙酸、EDTA-二钠、脲、三乙胺和氨。除了这些,无机酸如盐酸、磷酸、硫酸、硝酸和氢溴酸也可以使用。
显示酸度或碱度的聚合物也可以使用,其实例包括藻酸、聚谷氨酸、聚天冬氨酸、淀粉-丙烯酸接枝聚合物、聚丙烯酸酯(例如聚丙烯酸钠)、羧基乙烯基聚合物、乙酸乙烯酯/巴豆酸共聚物、乙酸乙烯酯/(甲基)丙烯酸共聚物、乙酸乙烯酯/巴豆酸共聚物、聚乙烯基磺酸、聚衣康酸、苯乙烯/马来酸酐共聚物和丙烯酰胺/丙烯酸共聚物,但是所述聚合物并不限于这些化合物。
为了提高水凝胶的保湿能力或增强抗坏血酸或其衍生物的效果,本发明水凝胶中可以加入溶剂等。可以使用的溶剂实例包括能与水混溶的有机溶剂如醇、酮(例如丙酮、甲乙酮)、溶纤剂、二恶烷、二甲基甲酰胺、N-甲基吡咯烷酮和二甲基亚砜,和与水不混溶的有机溶剂如乙酸乙酯和克罗他米通。
醇的实例包括一元醇,例如甲醇、乙醇、丙醇、苯甲醇、苯乙醇、异丙醇、异丁醇、己醇、2-乙基己醇、环己醇、辛醇、丁醇、乙二醇一丁基醚和戊醇;乙二醇、丙二醇、1,3-丁二醇、二甘醇、三甘醇、1,4-丁二醇(二元醇),甘油、三氧代异丁烷(三元醇);赤藻糖醇、季戊四醇(四元醇),木糖醇、戊五醇(五元醇),异半乳糖醇、山梨糖醇、液体山梨糖醇和甘露醇(六元醇),但是本发明并不仅限于此。其中,从对皮肤的刺激或保湿性着眼,优选多元醇。
在本发明水凝胶用作医药应用介质的情况下,药剂可与仍处于溶胶状态的水凝胶混合或混入熟化后的凝胶中。可根据药剂的性能以及有关给药部位和释放速率的原始目的选择适当方法。
大量的药剂可利用本发明水凝胶给药,其实例包括抗炎止痛药剂,例如水杨酸、水杨酸乙二醇酯、水杨酸甲酯、1-薄荷醇、樟脑、苏灵大、三次甲基钠、甲氧萘丙酸、联苯丁酮酸、吡氧噻嗪、醋酸去炎松、醋酸氢化可的松、吲哚美辛、酮丙酸、醋氨酚、甲灭酸、氟灭酸、对异丁基苯乙酸、洛索丙普、噻洛芬(thiaprofen)、普拉洛芬、芬普洛芬(fenpurofen)、双氯芬酸(dichlofenac)、双氯芬酸钠、烯氯苯乙酸、羟基保泰松、异丁苯丙酸、联苯乙酸、Ketronac、柏莫洛芬、Napmeton、甲氧萘丙酸、氟比洛芬、氟轻松和丙酸氯氟美松。
其它实例包括皮质类固醇激素、抗真菌剂、抗组胺剂、催眠镇静剂、镇定剂、抗高血压药剂、抑制利尿剂、抗生素、麻醉剂、抗菌物质、维生素制剂、抗癫痫药物、冠状血管扩张剂、抗组胺剂、止咳药、性激素、抗抑郁剂、咽痛处理剂、麻醉镇痛剂、天然药物、5-氟脲嘧啶、二氢麦角胺、芬太尼、去氨加压素(desmopressin)、地谷新、胃复安、哌双咪酮、东莨菪胺、东莨菪碱氢溴酸盐、用于动物的药剂、催眠药、循环系统处理剂、大脑代谢激活剂、杀菌剂、酶制剂、酶抑制剂、生物药剂(多肽)、角化症处理剂、镇静剂、抗肿瘤药、全身麻醉药、抗焦虑药、用于哮喘和鼻过敏的药物、抗帕金森氏综合症药物、化学处理剂、驱虫药、抗原生动物病药物、抗真菌剂(arthrifuges)、止血剂、强心剂、刺激性抗镇静剂、抗毒瘾药物、中草药、放射药剂、用于泌尿生殖系统和肛门的药物、降低血糖的药物、抗溃疡药剂、用于毛发的药物、隐蔽剂、发赤剂、抗汗剂、镇定剂、抗凝血剂、治疗风湿的药物、抗痛风药物和促凝药物,但是,本发明并不仅限于此。如果需要,这些药物可以两种或多种组合使用。
可以添加促进抗坏血酸或其衍生物吸收的辅助试剂,其实例包括角蛋白软化剂,例如乙醇、异丙醇、丁醇、1,3-丁二醇、丙二醇、聚乙二醇#400、甘油、克罗他米通、苯甲醇、苯基乙基醇、碳酸亚丙酯、己基十二烷醇、丙醇、尿囊素、二甲基亚砜、二甲基乙酰胺、二甲基甲酰胺、己二酸二异丙酯、癸二酸二乙酯、月桂酸乙酯、羊毛酯、氮酮、1-香叶基氮杂环庚-2-酮(GACH)、脂肪酸二羟烷基酰胺、水杨酸、水杨酸衍生物、脲和硫;润湿剂,例如吡咯烷酮羧酸;表面活性剂,例如丙二醇一油酸脂、聚氧乙烯山梨糖一硬脂酸酯、山梨糖一硬脂酸酯和甘油一硬脂酸酯;酯,例如肉豆蔻酸异丙酯和癸二酸二乙酯;高级醇,例如油醇、硬脂醇和月桂醇;脂肪酸,例如硬脂酸、己酸、壬酸、癸酸、十四烷酸、十六烷酸、十八烷酸、油酸和亚油酸:萜烯基化合物,例如薄荷醇、薄荷酮、1,8萜二烯、蒎烯、薄荷酮、萜品烯、萜品油烯、萜品油和香芹醇;油成分,例如杏仁油、橄榄油、山茶油、桃仁油、薄荷油、芝麻油、豆油、貂油、棉花籽油、玉米油、红花油、椰子油、桉树油、蓖麻油、液体石蜡、凡士林、角鲨烯、角鲨烷和羊毛酯。这些成分可一种或多种混合。从皮肤刺激等着眼,所述辅助剂的混合量优选为按每100质量份水凝胶计0.1-5质量份。
在本发明水凝胶中,可以组合使用其它活性成分,并且那些公知的活性成分可自由添加,例如抗粉刺剂、抗雄激素、杀菌剂、抗炎药剂、抗氧化剂、自由基清除剂和增白剂。可组合使用的抗雄激素活性成分的实例包括乙酸赛普龙、螺内酯、雄激素和肾上腺糖皮质激素;可组合使用的杀菌活性成分的实例包括抗生素,例如红霉素、氯洁霉素、庆大霉素、青霉素、氯霉素和四环素,和抗菌成分,例如过氧化苯甲酰、纳地沙星、乙醇、氯下烷铵(洁尔灭)、硫、对羟基苯甲酸酯、水杨酸、4异丙基环庚二烯酚酮、三氯森和氨下磺胺;可以组合使用的抗炎药实例包括皮考布洛芬、甘草甜素、樟脑和消炎痛。
可以组合使用的抗粉刺活性成分的实例包括维甲酸、间苯二酚、异丙基甲基酚、生育酚和抗坏血酸。组合使用增白剂的实例包括胎盘提取物、曲酸、鞣花酸、熊果酚甙和凝血酸酯。除此之外,可以组合使用源于植物的抗菌剂、抗菌和抗炎成分,例如甘菊提取物、熊世(sasa albo-marginata)提取物、玫瑰提取物、香膏薄荷提取物、龙胆提取物、干草提取物、加州希蒙得木提取物、迷迭香提取物、一串红提取物、百里香提取物、熏衣草提取物、芍药提取物、人参提取物、芦荟提取物、大豆提取物、紫苏提取物、艾属植物提取物、姜黄提取物、日本扁柏叶提取物、日本扁柏提取物、大黄提取物、黄柏皮提取物、日本黄连提取物、银杏树提取物、桑树皮提取物、绿茶提取物、柚子皮提取物、五加科提取物、七叶胆提取物和各种海藻提取物。所述组合使用活性成分的添加量为基于水凝胶的0.01-50质量%,但具体根据种类和使用成分而变化。
在本发明水凝胶中,为了更顺利地突出本发明水凝胶的特性,提高加工成型性能和质量,或提高抗坏血酸或其衍生物在本发明水凝胶中的分散性和稳定性,可进一步任意混入根据该目的选择的化合物,其混入程度应不损害本发明水凝胶的性能。
这些添加剂包括:
(1)增湿剂:例如,甘油、丙二醇、山梨糖醇、1,3-丁二醇、dl-吡咯烷酮羧酸和乳酸钠;
(2)收敛剂:例如,柠檬酸、酒石酸、乳酸、氯化铝、硫酸铝、尿囊素氯-羟基铝、尿囊素二羟基铝、苯酚硫酸铝、对苯酚磺酸锌、硫酸锌和羟基氯化铝;
(3)湿润剂:例如,多元醇如甘油、丙二醇、1,3-丁二醇、山梨糖醇、聚甘油、聚乙二醇和二丙二醇;NMF成分如乳酸钠;和水溶性聚合物如透明质酸、胶原质、黏多糖和硫酸软骨素;
(4)增稠剂:例如,天然聚合物如阿拉伯树胶、黄蓍胶、豆角胶、瓜尔胶、Echo gum、刺梧桐树胶、琼脂、淀粉、交叉菜胶、藻酸、藻酸盐(例如藻酸钠)、丙二醇藻酸酯、右旋糖苷、糊精、直链淀粉、明胶、胶原质、支链淀粉、胶质、胶淀粉、淀粉、胶淀粉半甘醇酸钠(sodium amylopectinsemiglycolate)、角素、白蛋白和酪蛋白;半合成聚合物,例如聚谷氨酸、聚天冬氨酸、甲基纤维素、乙基纤维素、丙基纤维素、乙基甲基纤维素、羟乙基纤维素、羟丙基纤维素、羟基-丙基甲基纤维素、羧甲基淀粉、碱金属羧甲基纤维素、碱金属纤维素硫酸盐、纤维素接枝聚合物、交联的明胶、邻苯二甲酸醋酸纤维素、淀粉-丙烯酸接枝共聚物、邻苯二甲酸酐改性的明胶和琥珀酸改性的明胶;合成聚合物,例如聚乙烯醇、聚乙烯基吡咯烷酮、聚乙烯基甲基醚、羧基乙烯基聚合物、乙烯基吡咯烷酮/丙烯酸乙酯共聚物、乙烯基吡咯烷酮/苯乙烯共聚物、乙烯基吡咯烷酮-乙酸乙烯酯共聚物、乙酸乙烯酯/(甲基)丙烯酸共聚物、乙酸乙烯酯/巴豆酸共聚物、N-乙烯基乙酰胺基共聚物(例如,N-乙烯基乙酰胺/丙烯酸钠共聚物)、交联N-乙烯基乙酰胺聚合物、聚衣康酸、聚丙烯酸羟基乙酯、聚丙烯酰胺、苯乙烯/马来酸酐共聚物和丙烯酰胺/丙烯酸共聚物;
(5)增粘物质:例如,增粘物质如硅橡胶、聚异戊二烯橡胶、苯乙烯嵌段共聚橡胶、丙烯酸橡胶和生橡胶;
(6)抗痒剂:例如,樟脑、百里酚、薄荷醇、聚氧乙烯月桂基醚、抗组胺剂和氨基苯甲酸乙酯;
(7)角蛋白软化剂和磨蚀剂:例如,硫、噻克索酮(thioxolone),硫化硒、水杨酸和间苯二酚;
(8)意外摄取预防物质:例如辣椒粉和辣椒精;
(9)粉末原料:例如,蒙脱石、硅酸酐、石膏、炭黑、硅藻土、氧化铁红、碳酸钙、水滑石、滑石、玻璃、高岭土、斑脱土、金属皂、高度分散的硅胶(aerosil)、钛酸盐云母、氯氧化铋、鱼鳞片、锌白和二氧化钛;
(10)油状原料:例如,杏仁油、橄榄油、硬化油、山茶油、蓖麻油、日本蜡油、椰子油、蜂蜡、鲸蜡、羊毛脂、巴西棕榈蜡、小烛树蜡、液体石蜡、凡士林、微晶蜡、地蜡、角鲨烯、月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、异硬脂酸、油酸、月桂醇、鲸蜡醇、硬脂醇、油醇、十八烷醇、胆固醇、己基正癸醇、白固醇(white sterol)、乳酸鲸蜡酯、肉豆蔻异丙酯、月桂酸己酯、肉豆蔻酸肉豆蔻酯、棕榈酸异丙酯、肉豆蔻酸辛基十二醇酯、硬脂酸丁酯、可可油、日本蜡、加州希蒙得木油、葡萄籽油、鳄梨油、貂油、蛋黄油、蜂蜡、鲸蜡、羊毛酯、巴西棕榈蜡、小烛树蜡、液体石蜡、地蜡、石蜡、山俞酸,己二酸异丙酯、肉豆蔻酸辛基十二烷基酯、油酸十二烷基酯和油酸胆固醇酯;
(11)表面活性剂:例如,阴离子表面活性剂如硫酸月桂酯、聚氧乙烯烷基醚硫酸酯、烷基苯磺酸酯、聚氧乙烯烷基醚磷酸、聚氧乙烯烷基苯基醚磷酸、N-酰基氨基酸盐、硬脂酸钠、棕榈酸钾、鲸蜡基硫酸钠、月桂基硫酸钠、三乙醇胺棕榈酸酯、聚氧乙烯月桂基磷酸钠、酰基谷氨酸钠和生物界面活性剂(Surfactin);阳离子表面活性剂如氯下烷铵(洁而灭)、苯索氯铵(benzetonium chloride)、氯化硬脂基-三甲基铵、氯化二硬脂基二甲基铵和氯化硬脂基二甲基苄基铵;两性表面活性剂,例如烷基二氨基甘氨酸盐酸化物、2-烷基-N-羧甲基-N-羟乙基-咪唑啉鎓甜菜碱、月桂基二甲基氨基乙酸甜菜碱和卵磷脂;非离子表面活性剂,例如多元醇脂肪酸酯、单硬脂酸甘油酯、亲油性单油酸甘油酯、单硬脂酸乙二醇酯、单硬脂酸丙二醇酯、脱水山梨醇脂肪酸酯、聚氧乙烯脱水山梨醇脂肪酸酯、聚氧乙烯脂肪酸酯、N-酰基氨基酸酯、脂肪酸糖酯、脂肪酸羟烷基酰胺、聚氧乙烯化固醇、聚氧乙烯化羊毛脂和聚氧乙烯氢化蓖麻油;
12)着色剂:例如,氧化铁黄、氧化铁红、氧化铁黑、佛青、炭黑、氢氧化铬、氧化铬、焦油颜料、色淀、食品红102、食品红201、食品黄4、食品黄5、食品蓝1和食品蓝2;
(13)香料:例如,植物香料如芥菜油、橙油、芝麻油、茉莉油、日本雪松油、鸢尾油、1,8萜二醇油、橙花油、玫瑰油、桉树油、酸橙油、柠檬油、日本薄荷油和迷迭香油;动物香料,例如麝香、香猫、海狸香和龙涎香;烃基香料如溴代苏合香烯、蒎烯和柠檬油精;醇基香料如苄基醇和1-薄荷醇;酯基香料如乙酸乙酯和水杨酸甲酯;醛基香料如苯甲醛和水杨醛;酮基香料如樟脑、麝香酮、麝香酮和1-薄荷酮;醚基香料如黄樟油精;酚基香料如麝香草酚;内酯基香料;酸基香料如苯乙酸;和氮化合物基香料如吲哚;
(14)紫外线屏蔽剂:例如,苯甲酮类型如ASL-24、Cyasorb UV-9和Uvinul M-40;苯甲酸类型如水杨酸苯酯(Salol);吡咯类型如Tinuvin P;腈类型如Uvinul N-35;脲类型如Ancour UA;对氨基酸类型如NeoHeliopan Give tan F、2-羟基-4-甲氧基苯甲酮、对氨基苯甲酸辛基二甲酯和对甲氧基肉桂酸乙基己基酯;水杨酸类型;苯并呋喃类型;香豆素类型;吡咯类型;
(15)防腐和杀菌剂:例如,酸如苯甲酸、水杨酸、脱氢乙酸、山梨酸和硼酸;这些酸的盐;酚如苯酚、氯甲酚、氯代二甲苯酚、异丙基甲基苯酚、间苯二酚、邻苯基苯酚、对羟基苯甲酸酯、苯氧乙醇、百里酚、4-异丙基环庚二烯酚酮和噻克索酮;卤化双酚如六氯酚和2,4,4′-三氯-2′-羟基联苯醚;酰胺化合物如三氯代N-碳酰苯胺、卤卡班和十一碳烯酸单乙醇酰胺;季铵化合物如氯化苯甲烃铵、溴化烷基异喹啉鎓、氯化苯甲乙氧铵和氯化鲸蜡基吡啶鎓;两性表面活性剂如月桂基二(氨基乙基)甘氨酸;2-吡啶硫醇-1-氧化锌盐;葡糖酸;双氯苯双胍己烷;二硫化四甲秋兰姆;N-三氯代甲基硫醇-4-环己烯-1,2-二羧酰亚胺;和氯代丁醇;
(16)抗氧化剂:例如,去甲二氢愈创木酸、愈创木脂、镓酸丙酯、丁基苯甲醚、二丁基羟基甲苯(BHT)、生育酚(维生素E)和2,2′-亚甲基二(4-甲基-6-叔丁基)苯酚;
(17)螯合剂:例如,乙二胺四乙酸盐、焦磷酸盐、偏磷酸己酯(hexameta-phosphate)、柠檬酸、酒石酸和葡糖酸;
(18)紫外线散射剂:例如,二氧化钛、高岭土和滑石;和
(19)溶剂:例如,水混溶性有机溶剂如酮(例如丙酮、甲乙酮)、溶纤剂、二恶烷、二甲基甲酰胺、N-甲基吡咯烷酮和二甲基亚砜;水不混溶性有机溶剂如乙酸乙酯和克罗他米通;以及醇如甲醇、乙醇、丙醇、苯甲醇、苯乙醇、异丙醇、异丁醇、己醇、2-乙基己醇、环己醇、辛醇、丁醇和戊醇。
另外,可以使用稳定剂、填料、防腐剂、增塑剂、软化剂、劣化抑制剂等,并且,这些添加剂可在不会对所得水凝胶性能产生不利影响的范围内自由添加。
当本发明水凝胶形成厚度0.5mm的薄膜时,在25℃和相对湿度60%条件下暴露24小时后,依照JIS Z0237粘着性测试方法在其表面测试粘着性,当倾斜角为30°时球式粘着值为10或更高。
制备本发明水凝胶的方法描述如下。
制备本发明水凝胶的方法包括制备包含下述成分的混合物:至少两种选自聚丙烯酸、聚丙烯酸钠和部分中和的聚丙烯酸酯中的聚合物,铝化合物,水和抗坏血酸或其衍生物;在25-60℃下加热该混合物。
加热温度优选为35-55℃,更优选40-50℃。如果加热温度低于25℃,则凝胶化需要较长时间,反之,如果加热温度高于65℃,则可能不能获得抗坏血酸或其衍生物的稳定性。
本发明水凝胶可例如通过下述方法制备:将抗坏血酸或其衍生物、铝化合物、水、聚丙烯酸等分散于多元醇中,在捏合该分散体的同时将其加入包含pH调节剂的水中,如果必要,加入其它添加剂,然后加热捏合后的材料。
在本发明生产方法中,水凝胶在混入交联剂后以溶胶状态成型并,如果必要的话,加热,从而进行后交联。或者,交联后使用适当的成型机、压片机等将水凝胶直接成型为各种形状的物品。顺便指出,在加热时,凝胶化速率被提高。
通过将适当量的本发明水凝胶涂覆到载体的一个表面或两个表面可以获得水凝胶片,其中所述载体为例如纸张,木材,金属,玻璃纤维,布(例如法兰绒、纺织物、无纺物),合成树脂(例如聚氨酯,乙烯/乙酸乙烯酯共聚物,聚氯乙烯,聚酯(例如聚对苯二甲酸乙二醇酯),聚烯烃(例如聚乙烯、聚丙烯)、聚酰胺(例如尼龙6、尼龙66),聚偏二氯乙烯,聚四氟乙烯),金属箔(例如铝),橡胶,纤维素衍生物,模制品如与塑料薄膜的层压薄膜,薄片(箔)或带。为了使所获得的片状水凝胶便于储存,优选将通过硅氧烷处理或通过其它适当方法处理的脱模片附着在用水凝胶涂覆的表面上,或者用硅氧烷或其它方法处理没有涂覆压敏黏合剂的表面以形成脱模表面,并且在没有涂覆凝胶的表面上滚动或重叠。可以使用的脱模片实例包括聚乙烯薄膜、聚丙烯薄膜、脱模纸、玻璃纸、聚氯乙烯和聚酯。
本发明将参照下述实施例和对比例作进一步阐述,但是,本发明并不局限于这些实施例。在实施例中,“份”为“质量份”。
实施例1
依照下述原料混合比例和配方制备水凝胶。
原料混合比例
聚丙烯酸钠 2份
丙烯酸/丙烯酸钠(50/50(摩尔))共聚物 2份
甘油 30份
氢氧化镁-氢氧化铝共沉淀物 1份
水 61份
二异丙醇胺 1份
抗坏血酸-2-磷酸镁 3份
配方
将抗坏血酸-2-磷酸镁(″抗坏血酸PM″,由ShowaDenko K.K.生产)、聚丙烯酸钠(″Viscomate F480SS″,由Showa Denko K.K.生产)、丙烯酸/丙烯酸钠(50/50(摩尔))共聚物(部分中和的聚丙烯酸酯)(″ViscomateNP-700″,由Showa Denko K.K.生产)和氢氧化镁-氢氧化铝共沉淀物(″Sanalmin″,由Kyowa Chemical Industry Co.,Ltd.生产)的甘油分散液捏合,同时将它们逐渐加入二异丙醇胺水溶液中。用刮刀式涂胶机以0.5mm的间隙将得到的溶胶涂布到聚丙烯衬垫上,然后将无纺织物黏附于该溶胶上,将其整体放入铝层压袋中并加热密封该袋。在熟化3天后,获得一种硬膏剂。当用手指触摸无纺织物上的凝胶时,该凝胶轻微伸长并显示强弹性。用纯化水稀释该凝胶100倍并测量pH,结果pH为8.2。另外,将得到的硬膏剂在25℃和相对湿度60%的条件下暴露24小时,然后依照JIS Z0237粘着性测试方法以30°的倾斜角测量球式粘着值,结果,球式粘着值为14。
实施例2
依照下述原料混合比例和配方制备水凝胶.
原料混合比例
聚丙烯酸钠 2份
丙烯酸/丙烯酸钠(70/30(摩尔))共聚物 2份
D-山梨糖醇溶液 30份
纯化水 61.5份
氢氧化铝 0.5份
氨基乙酸二羟基铝 0.5份
二异丙醇胺 0.5份
抗坏血酸-2-磷酸锌 3份
配方
将抗坏血酸-2-磷酸锌、聚丙烯酸钠、丙烯酸/丙烯酸钠(70/30(摩尔))共聚物(部分中和的聚丙烯酸酯)和氨基乙酸二羟基铝(″GLYCINAL″,由Kyowa Chemical Industry Co.,Ltd.生产)和氢氧化铝(“干燥氢氧化铝凝胶S-100”,由Kyowa Chemical Industry Co.,Ltd.生产)的D-山梨糖醇(70w/v%D-山梨糖醇水溶液)分散液捏合,同时将它们逐渐加入二异丙醇胺水溶液中。用刮刀式涂胶机以0.5mm的间隙将得到的溶胶涂布到聚丙烯脱模纸上,然后将无纺织物黏附于该溶胶上,将其整体放入铝层压袋中并加热密封该袋。在熟化3天后,获得一种硬膏剂。当用手指触摸无纺织物上的凝胶时,该凝胶轻微伸长并显示强弹性。按照与实施例1相同的方式测量该凝胶的pH,结果pH为8.5。另外,将得到的硬膏剂在25℃和相对湿度60%的条件下暴露24小时,然后依照JIS Z0237粘着性测试方法以30°的倾斜角测量球式粘着值,结果,球式粘着值为22。
实施例3
依照下述原料混合比例和配方制备水凝胶.
原料混合比例
聚丙烯酸钠 2份
丙烯酸/丙烯酸钠(80/20(摩尔))共聚物 2份
氢氧化镁-氢氧化铝共沉淀物 0.5份
氢氧化铝 0.5份
丙二醇 30份
纯化水 61份
抗坏血酸-2-磷酸钠 4份
配方
将抗坏血酸-2-磷酸钠(″抗坏血酸PS″,由ShowaDenko K.K.生产)、聚丙烯酸钠(″Viscomate F480SS″,由Showa Denko K.K.生产)、丙烯酸/丙烯酸钠(80/20(摩尔))共聚物(部分中和的聚丙烯酸酯)和氢氧化镁-氢氧化铝共沉淀物(″Sanalmin″,由Kyowa Chemical Industry Co.,Ltd.生产)和氢氧化铝(“干燥氢氧化铝凝胶S-100”,由Kyowa ChemicalIndustry Co.,Ltd.生产)的甘油分散液捏合,同时将它们逐渐加入水中。所得到的溶胶以0.5mm的间隙成型、密封、在50℃下熟化1天,然后从容器中取出以获得凝胶状包裹剂。当用手指触摸该凝胶时,该凝胶伸长并显示强弹性。按照与实施例1相同的方式测量凝胶的pH,发现pH为7.4。另外,将得到的包裹剂在25℃和相对湿度60%的条件下暴露24小时,然后依照JIS Z0237粘着性测试方法以30°的倾斜角测量球式粘着值,结果,球式粘着值为18。
实施例4
依照下述原料混合比例和配方制备水凝胶.
原料混合比例
丙烯酸钠/丙烯酸(80/20(摩尔))共聚物 10份
聚丙烯酸钠 10份
聚丙烯酸 10份
N-甲基-N-乙烯基乙酰胺/丙烯酸钾(60/40(重量))共聚物 1份
硅铝酸镁 5份
硫酸铝钾 5份
氢氧化纳 0.5份
乙醇 30份
水 28份
抗坏血酸-2-糖苷 0.5份
配方
将抗坏血酸-2-糖苷、聚丙烯酸钠(″Viscomate F480SS″,由ShowaDenko K.K.生产)、丙烯酸钠/丙烯酸(80/20(摩尔))共聚物(部分中和的聚丙烯酸酯)和聚丙烯酸、N-甲基-N-乙烯基乙酰胺共聚物和硅铝酸镁(″Neusilin″,由Fuji Chemical Industry Co.,Ltd.生产)的乙醇分散液一次全部加入包含氢氧化钠和硫酸铝钾的溶液中并捏合。所得到的溶胶以0.5mm的间隙成型、密封、在室温下熟化7天,然后从容器中取出以获得硬膏剂。当用手指触摸该凝胶时,该凝胶伸长并显示强弹性。按照与实施例1相同的方式测量凝胶的pH,发现pH为8.5。另外,将得到的硬膏剂在25℃和相对湿度60%的条件下暴露24小时,然后依照JIS Z0237粘着性测试方法以30°的倾斜角测量球式粘着值,结果,球式粘着值为15。
实施例5
原料混合比例
丙烯酸钠/丙烯酸(70/30(摩尔))共聚物 1份
聚丙烯酸 1份
N-乙烯基乙酰胺/丙烯酸钠(9/1(重量))共聚物 3份
纯化水 64.88份
氢氧化铝-碳酸氢钠共沉淀物 0.05份
乳酸铝 0.05份
1,3-丁二醇 30份
10%氨水 0.01份
抗坏血酸-2-磷酸镁 0.01份
配方
将抗坏血酸-2-磷酸镁(″抗坏血酸PM″,由Showa Denko K.K.生产)、丙烯酸钠/丙烯酸(70/30(摩尔))共聚物(部分中和的聚丙烯酸酯)(″ViscomateNP-600″,由Showa Denko K.K.生产)、聚丙烯酸、N-乙烯基乙酰胺/丙烯酸钠(9/1(重量))共聚物和氢氧化铝-碳酸氢钠共沉淀物(″Kumulite″,由Chemical Industry Co.,Ltd.)的1,3-丁二醇分散液捏合,同时将它们加入包含氨和乳酸铝的水溶液中。用刮刀式涂胶机以0.5mm的间隙将得到的溶胶涂布到聚丙烯衬垫上,然后将无纺织物黏附于该溶胶上,将其整体放入铝层压袋中并加热密封该袋。在熟化3天后,获得一种硬膏剂。当用手指触摸附着在无纺织物上的凝胶时,该凝胶轻微伸长并显示强弹性。按照与实施例1相同的方式测量凝胶的pH,发现pH为6.5。另外,将得到的硬膏剂在25℃和相对湿度60%的条件下暴露24小时,然后依照JIS Z0237粘着性测试方法以30°的倾斜角测量球式粘着值,结果,球式粘着值为10。
对比例1
原料混合比例
聚丙烯酸钠 4份
甘油 30份
纯化水 61份
氢氧化镁-氢氧化铝共沉淀物 1份
二异丙醇胺 1份
抗坏血酸-2-磷酸镁 3份
配方
将抗坏血酸-2-磷酸镁(″抗坏血酸PM″,由ShowaDenko K.K.生产)、聚丙烯酸钠(″Viscomate F480SS″,由Showa Denko K.K.生产)和氢氧化镁-氢氧化铝共沉淀物(″Sanalmin″,由Kyowa Chemical Industry Co.,Ltd.生产)的甘油分散液捏合,同时将它们逐渐加入二异丙醇胺水溶液中。用刮刀式涂胶机以0.5mm的间隙将得到的溶胶涂布到聚丙烯衬垫上,然后将无纺织物黏附于该溶胶上,将其整体放入铝层压袋中并加热密封该袋。在熟化3天后,获得一种硬膏剂。当用手指触摸无纺织物上的凝胶时,该凝胶没有显示任何弹性并且与手指粘连。另外,所述无纺织物完全被溶胶湿润。
对比例2
原料混合比例
丙烯酸钠/丙烯酸(70/30(摩尔))共聚物 4份
纯化水 61.5份
氨基乙酸二羟基铝 0.5份
干燥氢氧化铝凝胶 0.5份
D-山梨糖醇溶液 30份
二异丙醇胺 0.5份
抗坏血酸-2-磷酸锌 3份
配方
将抗坏血酸-2-磷酸锌、聚丙烯酸钠、丙烯酸钠/丙烯酸(70/30(摩尔))共聚物(部分中和的聚丙烯酸酯)和氨基乙酸二羟基铝(″GLYCINAL″,由Kyowa Chemical Industry Co.,Ltd.生产)和氢氧化铝(“干燥氢氧化铝凝胶S-100”,由Kyowa Chemical Industry Co.,Ltd.生产)的D-山梨糖醇(70w/v%D-山梨糖醇水溶液)分散液捏合,同时将它们逐渐加入二异丙醇胺水溶液中。用刮刀式涂胶机以0.5mm的间隙将得到的溶胶涂布到聚丙烯衬垫上,然后将无纺织物黏附于该溶胶上,将其整体放入铝层压袋中并加热密封该袋。在熟化3天后,获得一种硬膏剂。当用手指触摸该硬膏剂上的凝胶时,该凝胶没有显示任何弹性并与手粘连。另外,所述无纺织物全部被溶胶湿润。
工业适应性
正如前面所述,本发明水凝胶能够稳定保持抗坏血酸或其衍生物,具有高凝胶强度,显示出与被黏附物的良好粘合,不引起液体脱水收缩,并且具有简单组成便于制备。通过利用本发明水凝胶,可以提供能够使抗坏血酸或其衍生物在皮肤等上的效果最佳的化妆品材料和类似产品。
Claims (11)
1.一种用于外用医疗制剂和化妆品的包含凝胶、水和抗坏血酸或其衍生物的水凝胶,其中所述凝胶包含至少两种聚合物,所述聚合物包括部分中和的聚丙烯酸酯以及从聚丙烯酸和聚丙烯酸钠中选择的至少一种,所述聚合物用铝化合物交联,并且当所述水凝胶用纯化水稀释100倍时pH为6.5-8.5,其中所述铝化合物是选自氢氧化镁-氢氧化铝共沉淀物、氢氧化铝、氨基乙酸二羟基铝、硅铝酸镁、硫酸铝钾、氢氧化铝-碳酸氢钠共沉淀物、乳酸铝,和其中所述抗坏血酸或其衍生物是选自抗坏血酸、抗坏血酸-2-磷酸酯、抗坏血酸-2-焦磷酸酯、抗坏血酸-2-三磷酸酯、抗坏血酸-2-多磷酸酯、抗坏血酸-2,3-二磷酸酯、抗坏血酸-2,6-二磷酸酯、抗坏血酸-2-硫酸酯、抗坏血酸-6-棕榈酸酯、抗坏血酸-2,6-棕榈酸酯、抗坏血酸-2-葡糖苷、抗坏血酸-2-O-葡糖苷-6-棕榈酸酯、抗坏血酸-5,6-亚苄基酯、抗坏血酸-5,6-亚丙基酯以及它们的金属盐、铵盐、烷基和羟烷基取代的铵盐,并且所述铝化合物的含量为按每100质量份所述水凝胶计0.01-10质量份,所述抗坏血酸或其衍生物的含量为按每100质量份所述水凝胶计0.01-10质量份。
2.如权利要求1所述的水凝胶,其中pH为7.0-8.0。
3.如权利要求1或2所述的水凝胶,其中铝化合物是氢氧化镁-氢氧化铝共沉淀物。
4.如权利要求1所述的水凝胶,其中抗坏血酸衍生物是抗坏血酸-2-磷酸酯或其盐。
5.如权利要求1所述的水凝胶,其中所述水凝胶包含多元醇。
6.如权利要求1所述的水凝胶,其中当所述水凝胶形成厚度0.5mm的薄膜并在25℃和相对湿度60%下暴露24小时后依照JIS Z0237粘着性测试方法在其表面测试粘着性时,倾斜角为30°时的球式粘着值为10或更高。
7.一种制备如权利要求1-6项中任一项所述的水凝胶的方法,包括:
制备包含以下组分的混合物:至少两种聚合物,所述聚合物包括部分中和的聚丙烯酸酯以及从聚丙烯酸和聚丙烯酸钠中选择的至少一种;铝化合物;水;和抗坏血酸或其衍生物的混合物,
并在25-65℃下加热该混合物。
8.如权利要求7所述的制备水凝胶的方法,其中当所述水凝胶用纯化水稀释100倍时pH被调整为6.5-8.5。
9.如权利要求8所述的制备水凝胶的方法,其中pH被调整为7.0-8.0。
10.一种包含权利要求1-6中任一项所述的水凝胶的化妆材料。
11.一种包含权利要求1-6中任一项所述的水凝胶的外用制剂。
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CN103623457A (zh) * | 2013-12-09 | 2014-03-12 | 长春吉原生物科技有限公司 | 一种异形水凝胶功能敷料及其制备方法 |
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US20060165801A1 (en) | 2006-07-27 |
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HK1072062A1 (en) | 2005-08-12 |
TW200400048A (en) | 2004-01-01 |
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EP1513889A1 (en) | 2005-03-16 |
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AU2003243001A1 (en) | 2004-01-06 |
DE60320251T2 (de) | 2009-05-14 |
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US8580849B2 (en) | 2013-11-12 |
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