CN1339958A - 封装方法 - Google Patents
封装方法 Download PDFInfo
- Publication number
- CN1339958A CN1339958A CN00803807.4A CN00803807A CN1339958A CN 1339958 A CN1339958 A CN 1339958A CN 00803807 A CN00803807 A CN 00803807A CN 1339958 A CN1339958 A CN 1339958A
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- CN
- China
- Prior art keywords
- mixture
- oil
- water
- microcapsule
- alcohol
- 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.)
- Pending
Links
- 238000005538 encapsulation Methods 0.000 title description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 73
- 239000000203 mixture Substances 0.000 claims abstract description 72
- 239000003921 oil Substances 0.000 claims abstract description 49
- 239000003094 microcapsule Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 claims abstract description 34
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229930002875 chlorophyll Natural products 0.000 claims abstract description 33
- 235000019804 chlorophyll Nutrition 0.000 claims abstract description 33
- 229910052802 copper Inorganic materials 0.000 claims abstract description 33
- 239000010949 copper Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 31
- 239000011162 core material Substances 0.000 claims abstract description 24
- 239000000284 extract Substances 0.000 claims abstract description 16
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000005662 Paraffin oil Substances 0.000 claims abstract description 8
- 108010010803 Gelatin Proteins 0.000 claims description 9
- 239000008273 gelatin Substances 0.000 claims description 9
- 229920000159 gelatin Polymers 0.000 claims description 9
- 235000019322 gelatine Nutrition 0.000 claims description 9
- 235000011852 gelatine desserts Nutrition 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000010668 complexation reaction Methods 0.000 claims description 7
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 5
- 239000002480 mineral oil Substances 0.000 claims description 4
- 235000010446 mineral oil Nutrition 0.000 claims description 4
- 239000000499 gel Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 241001465754 Metazoa Species 0.000 claims description 2
- 210000004195 gingiva Anatomy 0.000 claims description 2
- 239000011814 protection agent Substances 0.000 claims description 2
- 239000010775 animal oil Substances 0.000 claims 1
- 239000010773 plant oil Substances 0.000 claims 1
- 235000019198 oils Nutrition 0.000 abstract description 41
- 238000005354 coacervation Methods 0.000 abstract description 5
- 235000019486 Sunflower oil Nutrition 0.000 abstract 1
- 230000008676 import Effects 0.000 abstract 1
- 239000002600 sunflower oil Substances 0.000 abstract 1
- 229960004756 ethanol Drugs 0.000 description 14
- 239000000047 product Substances 0.000 description 10
- -1 octyl group ester Chemical class 0.000 description 8
- 239000000606 toothpaste Substances 0.000 description 6
- 229940034610 toothpaste Drugs 0.000 description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 5
- 239000000872 buffer Substances 0.000 description 5
- 239000002775 capsule Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 230000002421 anti-septic effect Effects 0.000 description 4
- 239000007766 cera flava Substances 0.000 description 4
- 239000003086 colorant Substances 0.000 description 4
- HWDGVJUIHRPKFR-UHFFFAOYSA-I copper;trisodium;18-(2-carboxylatoethyl)-20-(carboxylatomethyl)-12-ethenyl-7-ethyl-3,8,13,17-tetramethyl-17,18-dihydroporphyrin-21,23-diide-2-carboxylate Chemical compound [Na+].[Na+].[Na+].[Cu+2].N1=C(C(CC([O-])=O)=C2C(C(C)C(C=C3C(=C(C=C)C(=C4)[N-]3)C)=N2)CCC([O-])=O)C(=C([O-])[O-])C(C)=C1C=C1C(CC)=C(C)C4=N1 HWDGVJUIHRPKFR-UHFFFAOYSA-I 0.000 description 4
- 230000001804 emulsifying effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229940079841 sodium copper chlorophyllin Drugs 0.000 description 4
- 235000013758 sodium copper chlorophyllin Nutrition 0.000 description 4
- 235000015112 vegetable and seed oil Nutrition 0.000 description 4
- 239000008158 vegetable oil Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 229920002125 Sokalan® Polymers 0.000 description 3
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 239000003082 abrasive agent Substances 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000007859 condensation product Substances 0.000 description 3
- 239000000551 dentifrice Substances 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 235000002639 sodium chloride Nutrition 0.000 description 3
- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- ZTHYODDOHIVTJV-UHFFFAOYSA-N Propyl gallate Chemical compound CCCOC(=O)C1=CC(O)=C(O)C(O)=C1 ZTHYODDOHIVTJV-UHFFFAOYSA-N 0.000 description 2
- INVGWHRKADIJHF-UHFFFAOYSA-N Sanguinarin Chemical compound C1=C2OCOC2=CC2=C3[N+](C)=CC4=C(OCO5)C5=CC=C4C3=CC=C21 INVGWHRKADIJHF-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Natural products OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 239000003925 fat Substances 0.000 description 2
- 235000019197 fats Nutrition 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- CGIGDMFJXJATDK-UHFFFAOYSA-N indomethacin Chemical compound CC1=C(CC(O)=O)C2=CC(OC)=CC=C2N1C(=O)C1=CC=C(Cl)C=C1 CGIGDMFJXJATDK-UHFFFAOYSA-N 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- 239000000546 pharmaceutical excipient Substances 0.000 description 2
- 230000035479 physiological effects, processes and functions Effects 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229960003975 potassium Drugs 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- AVTYONGGKAJVTE-OLXYHTOASA-L potassium L-tartrate Chemical compound [K+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O AVTYONGGKAJVTE-OLXYHTOASA-L 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
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 239000004302 potassium sorbate Substances 0.000 description 2
- 235000010241 potassium sorbate Nutrition 0.000 description 2
- 229940069338 potassium sorbate Drugs 0.000 description 2
- 210000000582 semen Anatomy 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 2
- 239000004299 sodium benzoate Substances 0.000 description 2
- 235000010234 sodium benzoate Nutrition 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- 239000002562 thickening agent Substances 0.000 description 2
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 2
- 229940088594 vitamin Drugs 0.000 description 2
- 235000013343 vitamin Nutrition 0.000 description 2
- 239000011782 vitamin Substances 0.000 description 2
- 229930003231 vitamin Natural products 0.000 description 2
- 150000003722 vitamin derivatives Chemical class 0.000 description 2
- DTOUUUZOYKYHEP-UHFFFAOYSA-N 1,3-bis(2-ethylhexyl)-5-methyl-1,3-diazinan-5-amine Chemical compound CCCCC(CC)CN1CN(CC(CC)CCCC)CC(C)(N)C1 DTOUUUZOYKYHEP-UHFFFAOYSA-N 0.000 description 1
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 description 1
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 description 1
- OSCJHTSDLYVCQC-UHFFFAOYSA-N 2-ethylhexyl 4-[[4-[4-(tert-butylcarbamoyl)anilino]-6-[4-(2-ethylhexoxycarbonyl)anilino]-1,3,5-triazin-2-yl]amino]benzoate Chemical compound C1=CC(C(=O)OCC(CC)CCCC)=CC=C1NC1=NC(NC=2C=CC(=CC=2)C(=O)NC(C)(C)C)=NC(NC=2C=CC(=CC=2)C(=O)OCC(CC)CCCC)=N1 OSCJHTSDLYVCQC-UHFFFAOYSA-N 0.000 description 1
- XBSLKMQADAAKGP-UHFFFAOYSA-N 2-hydroxypropane-1,2,3-tricarboxylic acid;phosphane Chemical compound P.OC(=O)CC(O)(C(O)=O)CC(O)=O XBSLKMQADAAKGP-UHFFFAOYSA-N 0.000 description 1
- FPPBCRLXUHYGHR-UHFFFAOYSA-N 2-tert-butyl-3-hydroxycyclohexa-2,5-diene-1,4-dione Chemical compound CC(C)(C)C1=C(O)C(=O)C=CC1=O FPPBCRLXUHYGHR-UHFFFAOYSA-N 0.000 description 1
- XGRSAFKZAGGXJV-UHFFFAOYSA-N 3-azaniumyl-3-cyclohexylpropanoate Chemical compound OC(=O)CC(N)C1CCCCC1 XGRSAFKZAGGXJV-UHFFFAOYSA-N 0.000 description 1
- PXRKCOCTEMYUEG-UHFFFAOYSA-N 5-aminoisoindole-1,3-dione Chemical compound NC1=CC=C2C(=O)NC(=O)C2=C1 PXRKCOCTEMYUEG-UHFFFAOYSA-N 0.000 description 1
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- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose 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](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 description 1
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- GHXZTYHSJHQHIJ-UHFFFAOYSA-N Chlorhexidine Chemical compound C=1C=C(Cl)C=CC=1NC(N)=NC(N)=NCCCCCCN=C(N)N=C(N)NC1=CC=C(Cl)C=C1 GHXZTYHSJHQHIJ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及用一种由至少90wt%C2～C4醇与水构成的混合物以一定浓度处理液体油与叶绿素铜提取物的混合物的方法。如此处理的混合物适合用络合凝聚来制造具有包含所述混合物的绿色液体芯材料的微胶囊。该微胶囊可加入到口腔护理产品中以赋予其彩色斑点外观。该液体油一般为向日葵油或石蜡油;C2～C4醇通常是乙醇或异丙醇。
Description
本发明涉及用溶剂处理油与叶绿素铜(copper chlorophyll)提取物的混合物以便使此种混合物适合例如制造含有含油与叶绿素铜混合物的液体芯材料的微胶囊的方法，所述微胶囊尤其适合用于，例如口腔护理产品。
以前，技术上曾建议将包含油芯和着色剂的微胶囊加入到口腔护理产品中，主要目的在于赋予该制品某种“有斑点的”(speckled)着色效果。譬如，GB-A-1，381，444(Blendax)描述一种微胶囊，它具有透明外壳材料，里面囊封着由彩色物质在诸如石蜡油之类生理惰性溶剂中的溶液或悬浮液。这些微胶囊可加入到牙膏中，以便为牙膏提供着色斑点效果。该着色材料是着色剂或颜料如各种各样红颜色、蓝颜色和绿颜色，绿颜色中又包括“绿颜色8(C-green 8)”，它是叶绿素铜络合物与叶绿酸铜的混合物。此种微胶囊可按熟知的囊封方法，如凝聚，以诸如明胶作为囊封材料来制造。
然而，我们发现，当用叶绿素铜作为着色剂时，按此种先有技术建议不能获得可接受的微胶囊。将叶绿素铜溶解在石蜡油中，当其加入到水中时将产生发黑的小颗粒，从而使该混合物不适合按凝聚法制取可接受的微胶囊。
在EP-A-0,711,544(Kao)中，描述了一种用于牙粉组合物的微胶囊，它包含琼脂作为包衣-形成材料，以及可由各种各样牙粉成分及其赋形剂构成的芯材料。在这些牙粉成分当中，也提到叶绿素铜；在赋形剂当中提到天然脂肪和油以及矿物油。虽然提到各种各样生产方法，包括凝聚，但优选采用双层喷嘴滴落方法来制造微胶囊。
在某些工作实例中，所描述的微胶囊包含，作为芯材料，一种中等链长甘油三酸酯和铜叶绿酸钠。
然而，铜叶绿酸钠可溶于水，于是我们发现，按该先有技术建议通过凝聚法无法获得含油与铜叶绿酸钠的芯的可接受微胶囊。乳化步骤期间，在油/水界面形成绿色淤浆，从而妨碍胶囊壁的形成。当采用叶绿素铜代替铜叶绿酸钠时，发现情况也是一样。
叶绿素提取物一般是通过对植物叶如苜蓿、草、荨麻属植物进行恰当萃取获得的。该萃取物一般包含叶绿素a和b，以及许多其他成分如颜料、碳水化合物、蜡、脂肪、油、盐、蛋白质以及叶黄素。
叶绿素铜萃取物的制备一般是通过在叶绿素提取物中以铜置换位于卟啉环中心的镁离子而实现的。
工业级叶绿素铜提取物(INCI名称：叶绿酸-铜络合物或CI75810；EINECS号234-242-5)通常是叶绿素铜提取物与植物油的混合物，最高含叶绿素铜15％。
现在，我们完全意外地发现，通过以至少90wt％的可以任意比例与水混溶的C2～C4一元醇与其余数量水的混合物处理叶绿素铜提取物与油的混合物，随后分离所形成的醇层和油层，便可获得一种含油和叶绿素铜的混合物，它完全适合采用凝聚方法制造含所述混合物的液体芯材料的完全合格微胶囊。这样的微胶囊包含绿色液体芯，以及透明或半透明外壳，从而为包含它们的口腔护理产品提供有斑点的外观，不会造成此种口腔护理产品使用时出现难看的胶囊皮进裂。优选的是，使用一种由至少96wt％可以任意比例与水混溶的C2～C4一元醇与其余数量的水构成的混合物。C2～C4一元醇的适宜例子是乙醇、丙醇、异丙醇、丁醇、异丁醇、叔丁醇和它们的混合物。优选的是乙醇和异丙醇，尤其优选乙醇。我们发现，最佳效果是当采用97.5％无水乙醇/2.5％水时获得的；借此可成功地处理在油中多至10％的叶绿素铜提取物。
上述工业级叶绿素铜是适用于本发明方法的原料。自然，也可将由其他来源取得的所需数量的叶绿素铜与油混合以获得所要求的原料。
虽然可以首先以醇/水混合物处理该含油工业级叶绿素铜提取物，然后回收含油和叶绿素铜的油层，再将所述层与油混合，但优选的是，首先将此种工业级提取物与适当的油混合，然后按本发明方法处理所述混合物。
于是，就典型而言，叶绿素铜/油混合物与醇/水混合物按2∶1～1∶4的比例(表示为叶绿素铜/油混合物的份数∶醇/水混合物的份数)，优选1份叶绿素铜/油混合物∶2份醇/水混合物，优选在剧烈搅拌下进行混合。所获混合物随后静置，直至出现相分离(分层)，一般至少要12h。所获绿色油相随后与含醇相分开，再次与相同比例的醇/水混合物进行混合，静置，直至相分离，一般要至少6h。所获绿色油相随后以水洗涤，以便除掉痕量醇。
如此获得的绿色油，随后与液体油混合，从而形成按凝聚方法成形微胶囊所需要的液体芯材料。该液体油可选自众所周知的液体植物油或动物食用油，例如豆油、菜籽油、棉籽油、椰子油、棕榈油、棕榈仁油、向日葵油、花生油、红花油、鱼油、鲸油等，以及它们的合成类似物，还有脂肪酸的甘油单酯和/或二酯。该液体油也可以是惰性、生理可接受的矿物油，如石蜡油。该液体油在等于或低于封装温度时，一般在等于或低于60℃，优选在等于或低于25℃时应呈液体或是可液化的。这些各种各样油的混合物也可使用。尤其优选的油是向日葵油。所获混合物的粘度不应过高或过低，否则凝聚方法将不能产生可接受的微胶囊。该粘度一般不应超过5Pa.s并且不低于0.004Pa.s。如果需要的话，该粘度可通过加入少量增稠剂，例如最高5％蜂蜡或蜂蜡酯或者增稠性二氧化硅，予以调节。
油/叶绿素铜混合物与液体芯油一般按1∶5～1∶1000、优选1∶10～1∶50的重量比彼此掺混以形成用于微胶囊的液体芯材料。
液体芯材料还可包含少量牙龈保键剂(gum health agent)如抗微生物剂，像玉洁纯；维生素、酶、角蛋白；还有调味油、防腐剂如苯甲酸钠和钾，抗氧剂如丁基化羟基甲苯(BHT)、丁基化羟基苯甲醚(BHA)、没食子酸丙基酯、辛基酯、十二烷基酯，叔丁基氢醌(TBHQ)(t-butylhydroxyquinone)、棕榈酸抗坏血酸酯、迷迭香油；油结晶抑制剂如卵磷脂或醇脂肪酸酯，也可包括在内。
微胶囊是通过熟知的凝聚方法制造的。凝聚是通过从亲水溶胶中盐析从而形成粘稠液滴形式的液态聚集体的过程。当2种带有相反电荷的亲水溶胶，例如明胶和阿拉伯树胶以恰当的数量混合在一起时，此种液滴或凝聚物最容易形成。
按照本发明优选的是，用明胶与阿拉伯树胶的混合物，优选交联的，例如以戊二醛为交联剂，来形成微胶囊的外壳。优选采用络合凝聚方法(complex coacervation)。液体芯材料用温热(40～60℃)明胶水溶液乳化。向该乳液中加入阿拉伯树胶和水，并将水相的pH值调节到4.0～4.5。水相优选包含防腐剂，如山梨酸钾。这将导致明胶、阿拉伯树胶和水的络合凝聚物的生成，并吸附在液体芯材料表面，于是围绕着分散的芯材料形成膜，从而形成微胶囊。随后，该体系冷却至通常低于10℃的温度，以便使凝聚物外壳固化。继而再加入戊二醛，使外壳交联。
此后，该微胶囊的含水淤浆可直接使用，或者经干燥后形成自由流动粉末。如此获得的微胶囊的大小通常在200～2000μm范围。该微胶囊可具有透明或半透明外壳，以及着绿色的液体或低熔点固体芯，从而使它们很容易在口腔护理产品中被看到。
微胶囊在口腔护理产品中的用量通常在0.1～5wt％，优选0.5～4wt％，一般介于1～3wt％。
可加入微胶囊的口腔护理产品可以是任何熟知的类型，例如膏体和凝胶。凝胶型是优选的，这样可以使微胶囊更容易可见，从而赋予该凝胶型口腔护理产品以诱人的美丽彩色斑点外观。
口腔护理组合物可包含任选的传统成分，例如药用上可接受载体，如淀粉、蔗糖、水或水/醇体系等。少量表面活性剂也可包括在内，例如阴离子、非离子、阳离子以及两性离子或两性表面活性剂。它们可包含颗粒状磨料，例如二氧化硅、氧化铝、碳酸钙、磷酸二钙、焦磷酸钙、羟基磷灰石、三偏磷酸盐、不溶性六偏磷酸盐等等，包括附聚的颗粒状磨料，一般用量介于3～60wt％。另外，还可包括水溶性温和磨料盐，如碳酸氢钠和碳酸钠。
此外，它们还可包含保湿剂，例如甘油、山梨醇、丙二醇、木糖醇、乳糖醇等。
粘结剂和增稠剂，如羧甲基纤维素钠、黄原酸胶、阿拉伯树胶，也可包括在内，还有合成聚合物，例如聚丙烯酸酯和羧乙烯基聚合物如丙烯酸聚合物(Carbopol)。
香料，如薄荷油及荷兰薄荷油，也可包括在内，还有防腐剂如苯甲酸钠，不透明剂，着色剂、pH-调节剂，缓冲剂如柠檬酸钾和酒石酸钾，香化剂以及诸如此类。
抗菌剂也可包括在内，例如三氯生、氯己定、铜-、锌-和亚锡盐，例如柠檬酸锌、柠檬酸钠锌和焦磷酸亚锡、血根碱提取物、甲硝唑。抗菌剂的另一些例子是季铵化合物，例如十六烷基氯化吡啶鎓；双胍，例如葡萄糖酸洗必太、海克替啶、奥替尼啶、阿来西定；卤化双酚化合物，如2，2’-亚甲基双-(4-氯-6-溴酚)。
可改善诸如抗菌剂之类有效成分的释放的聚合化合物也可包括在内。此类聚合物的例子是聚乙烯基甲基醚与马来酐的共聚物，以及其他类似的改善释放的聚合物，例如DE-A-3，942，643(Colgate)所描述的那些。
另外，消炎剂如布洛芬、氟比洛芬、阿司匹林、吲哚美辛等，也可包括在内。
防龋剂，例如氟化钠和氟化亚锡、氨氟化物(aminefluorides)、单氟磷酸钠、酪蛋白；牙菌斑缓冲剂(buffers)，例如尿素、乳酸钙、甘油磷酸钙、聚丙烯酸锶，也可包括在内。其他任选成分包括维生素，例如维生素C，以及植物提取物。另外脱敏剂如甘油单油酸酯、柠檬酸钾、氯化钾、酒石酸钾、碳酸氢钾、草酸钾、硝酸钾，乃至锶盐，也可包括在内。
用于缓冲组合物的pH值和离子强度的缓冲剂和盐也可包括在内。
另外，该口腔组合物也可包含防结石剂，例如焦磷酸碱金属盐、含次磷酸盐(hypophosphite)的聚合物、有机膦酸酯、磷柠檬酸盐(phosphocitrates)等。
此外，该组合物还可包含功能生命分子，如杆菌素、抗体、酶以及诸如此类的东西。
其他可包括的任选成分是，例如漂白剂如过氧化合物，如过氧二磷酸钾、泡腾体系如碳酸氢钠/柠檬酸体系，变色体系，以及诸如此类的。
该牙膏也可配制成双室型给药器使用的体系。
本发明将通过实例做进一步说明。在所有实例中，原料均为供应商供货形式的叶绿素铜提取物(13％叶绿素铜在植物油中的溶液)。随后，用向日葵油稀释到10倍，从而获得含1.3％叶绿素铜提取物的植物油与向日葵油的混合物。该混合物以下被称之为“混合物”。
实例1
混合物与97.5％乙醇/2.5％去离子水(1份油混合物：约2份乙醇/水)在分液漏斗中剧烈混合约1min，间歇地打开旋塞，以便让乙醇蒸汽跑出。所获混合物静置6h。随后，从分液漏斗中放出绿色油相，并令其与相同比例乙醇/水混合物再次混合，并静置3h。将如此获得的绿色油相放出并用水洗涤以除去残留痕量乙醇。如此获得的绿色油随后与向日葵油混合，混合比控制在，使最终混合物含有0.5wt％的原料供货起始浓度的叶绿素铜。该最终混合物被用作按下述络合凝聚方法制造含有它们的微胶囊的液体芯材料。该液体芯材料放在温热(50℃)明胶水溶液中进行分散和乳化。在该乳液中加入阿拉伯树胶和水，水相的pH值用乙酸调节到4.8。所获混合物慢慢冷却至室温，随后加入戊二醛。获得一种60％微胶囊在水中的含水淤浆。使用的明胶和阿拉伯树胶的数量控制在，使微胶囊外壳由50∶50明胶与阿拉伯树胶混合物组成(在产品中各占1.5％)，再以戊二醛交联。在此络合凝聚过程期间，加入0.5％山梨酸钾作为防腐剂。该微胶囊的平均直径为900μm，包括透明外壳和绿色液体芯。
实例2
混合物与96％乙醇/4％去离子水在分液漏斗中摇动约1min，间歇地打开旋塞，以便让乙醇蒸汽跑出。所获混合物静置6h。随后，从分液漏斗中放出形成的绿色油相，残留在乙醇层中的物质沉淀出来。当用水乳化时，该油层与水之间形成清晰界面，并发现适合在络合凝聚方法中用于成形微胶囊。然而，该油相的粘度却变得比原来略微下降，带有一定的乙醇气味，因此使该微胶囊用于口腔护理产品不太受青睐。
实例3
重复实例1，只是将经乙醇处理后获得的绿色油相与一种石蜡油混合，混合比例控制在，使最终液体芯材料包含5％向日葵油，从而制成与实例1类似的微胶囊。
重复该实例，但采用预先用2.5％蜂蜡或2.5％蜂蜡酯增稠的半软甘油三酸酯或向日葵油来代替石蜡油，所制成的微胶囊有些不透明，并且比实例1或按本实例3但用石蜡油所获得的，看上去要逊色。
实例4
混合物按类似于实例3的方式处理，但采用各种不同乙醇/水浓度。最后获得的乙醇/水相按分光光度法分析，采用540nm的波长做透明度评估。获得的结果如下：
乙醇/水浓度(％) λ＝540nm的吸光度对照例(未处理的混合物+矿物油) 0.2245
85/15 0.1380
90/10 0.0995
92.5/7.5 0.0935
95/5 0.0700
97.5/2.5 0.0595
100/0 0.0810
该结果表明，用97.5/2.5乙醇/水获得的含水乙醇相最透明。
实例5
在传统凝胶型牙膏中，加入1％实例1的微胶囊。所获牙膏具有诱人的绿色斑点外观。消费者调查结果显示，用此种牙膏获得的泡沫程度令人满意。
Claims (13)
1.一种用于处理液体油与叶绿素铜提取物的混合物的方法，以使所述混合物适合用于制造具有包含所述混合物的液体芯材料的微胶囊，其特征在于，所述混合物与一种由至少90wt％的可以任意比例与水混溶的C2～C4一元醇以及其余数量的水构成的混合物进行掺混，使所获混合物形成醇层和油层，并将油层与醇层分开。
2.权利要求1的方法，其特征在于，分离出的油层再用由至少90wt％的可以任意比例与水混溶的C2～C4一元醇以及其余数量的水构成的混合物处理，再次使所获混合物形成醇层和油层，并将油层与醇层分开。
3.权利要求1或2的方法，其特征在于，采用一种由至少96wt％的可以任意比例与水混溶的C2～C4一元醇以及其余数量的水构成的混合物。
4.权利要求1～3的方法，其特征在于，采用乙醇或异丙醇。
5.权利要求4的方法，其特征在于采用97.5％乙醇/2.5％水。
6.一种通过络合凝聚来制造含液体芯材料的微胶囊的方法，其特征在于，液体芯材料包含按权利要求1～5的方法制取的含叶绿素铜的油。
7.权利要求6的方法，其特征在于，液体芯材料包含液态或可液化的植物、动物或矿物油与按权利要求1～5的方法制取的含叶绿素铜油的混合物。
8.权利要求7的方法，其特征在于，混合物包含向日葵油或石蜡油。
9.权利要求6～8的方法，其特征在于，络合凝聚是采用明胶与阿拉伯树胶混合物作为微胶囊的成壳剂实施的。
10.权利要求9的方法，其特征在于，微胶囊用戊二醛进行处理。
11.权利要求6～10的方法，其特征在于，液体芯材料还包含牙龈保键剂。
12.口腔护理产品，它包含按权利要求6～11的方法获得的微胶囊。
13.权利要求12的口腔护理产品，其特征在于，该产品为凝胶形式。
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| JPS55161863A (en) * | 1979-06-06 | 1980-12-16 | Paaku Deebisu Kk | Colored gelatin capsule |
| US4224346A (en) * | 1979-06-15 | 1980-09-23 | International Flavors & Fragrances Inc. | Chewing gum composition containing one or more 2-oxabicyclooctane derivatives |
| SU955929A1 (ru) * | 1980-09-24 | 1982-09-07 | Всесоюзный научно-исследовательский институт синтетических и натуральных душистых веществ | Способ получени производных хлорофилла |
| JPS62125369A (ja) * | 1985-11-26 | 1987-06-06 | Mita Ind Co Ltd | 緑色トナ− |
| US4797392A (en) * | 1987-01-27 | 1989-01-10 | Chernomorsky Simon A | Use of anorectal compositions |
| US5077053A (en) * | 1990-02-12 | 1991-12-31 | Warner-Lambert Company | Zein as a moisture barrier for sugarless edible compositions and method for preparing same |
| RU2034555C1 (ru) * | 1992-02-13 | 1995-05-10 | Акционерное общество закрытого типа "Химико-биологическое объединение при РАН" | Экстрагент биоактивных компонентов из растительного сырья |
| TW412425B (en) * | 1994-10-18 | 2000-11-21 | Kao Corp | Dentifrice composition having capsule particles |
-
2000
- 2000-02-01 AU AU28000/00A patent/AU2800000A/en not_active Abandoned
- 2000-02-01 WO PCT/EP2000/000752 patent/WO2000048560A1/en not_active Application Discontinuation
- 2000-02-01 CN CN00803807.4A patent/CN1339958A/zh active Pending
- 2000-02-01 BR BR0008235-0A patent/BR0008235A/pt not_active Application Discontinuation
- 2000-02-01 EP EP00906252A patent/EP1152739A1/en not_active Ceased
- 2000-02-14 AR ARP000100621A patent/AR022585A1/es unknown
- 2000-02-14 US US09/503,920 patent/US6287542B1/en not_active Expired - Fee Related
-
2001
- 2001-08-03 ZA ZA200106409A patent/ZA200106409B/xx unknown
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100462067C (zh) * | 2007-02-15 | 2009-02-18 | 河北理工大学 | 铁叶绿酸钠-乙基纤维素微胶囊的制备方法 |
| CN107080708A (zh) * | 2017-03-30 | 2017-08-22 | 广州善草纪化妆品有限公司 | 一种温和多效洁面组合物 |
| CN107080708B (zh) * | 2017-03-30 | 2020-04-03 | 广州善草纪化妆品有限公司 | 一种温和多效洁面组合物 |
Also Published As
| Publication number | Publication date |
|---|---|
| AU2800000A (en) | 2000-09-04 |
| AR022585A1 (es) | 2002-09-04 |
| ZA200106409B (en) | 2002-08-05 |
| WO2000048560A1 (en) | 2000-08-24 |
| BR0008235A (pt) | 2001-10-30 |
| US6287542B1 (en) | 2001-09-11 |
| EP1152739A1 (en) | 2001-11-14 |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |