KR102588162B1 - Oral preparations containing water-soluble chitosan and manufacturing method thereof - Google Patents
Oral preparations containing water-soluble chitosan and manufacturing method thereof Download PDFInfo
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- KR102588162B1 KR102588162B1 KR1020230035159A KR20230035159A KR102588162B1 KR 102588162 B1 KR102588162 B1 KR 102588162B1 KR 1020230035159 A KR1020230035159 A KR 1020230035159A KR 20230035159 A KR20230035159 A KR 20230035159A KR 102588162 B1 KR102588162 B1 KR 102588162B1
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- water
- chitosan
- soluble chitosan
- deacetylation
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- 229920001661 Chitosan Polymers 0.000 title claims abstract description 135
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 35
- 230000006196 deacetylation Effects 0.000 claims abstract description 64
- 238000003381 deacetylation reaction Methods 0.000 claims abstract description 64
- 239000002324 mouth wash Substances 0.000 claims abstract description 57
- 229940051866 mouthwash Drugs 0.000 claims abstract description 52
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 16
- 241000241413 Propolis Species 0.000 claims abstract description 8
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims abstract description 8
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229940069949 propolis Drugs 0.000 claims abstract description 8
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims abstract description 8
- 229930182490 saponin Natural products 0.000 claims abstract description 8
- 150000007949 saponins Chemical class 0.000 claims abstract description 8
- 239000000811 xylitol Substances 0.000 claims abstract description 8
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims abstract description 8
- 229960002675 xylitol Drugs 0.000 claims abstract description 8
- 235000010447 xylitol Nutrition 0.000 claims abstract description 8
- 102000004190 Enzymes Human genes 0.000 claims abstract description 3
- 108090000790 Enzymes Proteins 0.000 claims abstract description 3
- 244000228451 Stevia rebaudiana Species 0.000 claims abstract description 3
- 229940088598 enzyme Drugs 0.000 claims abstract description 3
- 229940094952 green tea extract Drugs 0.000 claims abstract description 3
- 235000020688 green tea extract Nutrition 0.000 claims abstract description 3
- HELXLJCILKEWJH-NCGAPWICSA-N rebaudioside A Chemical compound O([C@H]1[C@H](O)[C@@H](CO)O[C@H]([C@@H]1O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)O[C@]12C(=C)C[C@@]3(C1)CC[C@@H]1[C@@](C)(CCC[C@]1([C@@H]3CC2)C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O HELXLJCILKEWJH-NCGAPWICSA-N 0.000 claims abstract description 3
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 42
- 230000000844 anti-bacterial effect Effects 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000007864 aqueous solution Substances 0.000 claims description 16
- 238000006386 neutralization reaction Methods 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- 239000011575 calcium Substances 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 230000002829 reductive effect Effects 0.000 claims description 3
- 230000001112 coagulating effect Effects 0.000 claims description 2
- 230000000087 stabilizing effect Effects 0.000 claims description 2
- 238000009472 formulation Methods 0.000 claims 1
- 230000008014 freezing Effects 0.000 claims 1
- 238000007710 freezing Methods 0.000 claims 1
- 206010006326 Breath odour Diseases 0.000 abstract description 17
- 230000036541 health Effects 0.000 abstract description 9
- 239000004615 ingredient Substances 0.000 abstract description 8
- 208000006558 Dental Calculus Diseases 0.000 abstract description 5
- 230000003239 periodontal effect Effects 0.000 abstract description 4
- 230000002087 whitening effect Effects 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000002265 prevention Effects 0.000 abstract description 3
- 230000000397 acetylating effect Effects 0.000 abstract description 2
- 241000894006 Bacteria Species 0.000 description 15
- 208000028169 periodontal disease Diseases 0.000 description 11
- 239000000126 substance Substances 0.000 description 9
- 208000002925 dental caries Diseases 0.000 description 8
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 239000000284 extract Substances 0.000 description 6
- 208000025157 Oral disease Diseases 0.000 description 5
- 208000030194 mouth disease Diseases 0.000 description 5
- 229920002101 Chitin Polymers 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 4
- 201000010099 disease Diseases 0.000 description 4
- 239000003995 emulsifying agent Substances 0.000 description 4
- 230000009931 harmful effect Effects 0.000 description 4
- 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 3
- 229960003260 chlorhexidine Drugs 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 210000000214 mouth Anatomy 0.000 description 3
- 229940034610 toothpaste Drugs 0.000 description 3
- 239000000606 toothpaste Substances 0.000 description 3
- 241000194019 Streptococcus mutans Species 0.000 description 2
- 235000019606 astringent taste Nutrition 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 206010013781 dry mouth Diseases 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 244000052769 pathogen Species 0.000 description 2
- 230000001717 pathogenic effect Effects 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 208000003265 stomatitis Diseases 0.000 description 2
- 230000009747 swallowing Effects 0.000 description 2
- 229920003169 water-soluble polymer Polymers 0.000 description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical group CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 1
- 241000238017 Astacoidea Species 0.000 description 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- 241000238557 Decapoda Species 0.000 description 1
- 208000002064 Dental Plaque Diseases 0.000 description 1
- 201000004624 Dermatitis Diseases 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 241000605986 Fusobacterium nucleatum Species 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 241000186660 Lactobacillus Species 0.000 description 1
- 208000003445 Mouth Neoplasms Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 241000519995 Stachys sylvatica Species 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 208000014151 Stomatognathic disease Diseases 0.000 description 1
- 241000194017 Streptococcus Species 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 230000021736 acetylation Effects 0.000 description 1
- 238000006640 acetylation reaction Methods 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 239000004599 antimicrobial Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000008376 breath freshener Substances 0.000 description 1
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 239000002781 deodorant agent Substances 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000019700 dicalcium phosphate Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000008029 eradication Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 230000002496 gastric effect Effects 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000005802 health problem Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000005934 immune activation Effects 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 208000012987 lip and oral cavity carcinoma Diseases 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000013588 oral product Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229940088417 precipitated calcium carbonate Drugs 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000035755 proliferation Effects 0.000 description 1
- 210000003296 saliva Anatomy 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 235000019605 sweet taste sensations Nutrition 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 235000019640 taste Nutrition 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
- 239000010913 used oil Substances 0.000 description 1
- 230000008673 vomiting Effects 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/736—Chitin; Chitosan; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/345—Alcohols containing more than one hydroxy group
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/98—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
- A61K8/987—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of species other than mammals or birds
- A61K8/988—Honey; Royal jelly, Propolis
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Microbiology (AREA)
- Emergency Medicine (AREA)
- Biotechnology (AREA)
- Mycology (AREA)
- Zoology (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Molecular Biology (AREA)
- Botany (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Cosmetics (AREA)
Abstract
키토산을 아세틸화하여 수용화 시킨 수용성 키토산 성분과 인체에 유익한 천연원료 성분을 핵심성분으로 활용함으로써, 구취제거, 치주관리, 미백, 치석관리 등 구강건강의 예방 및 관리에 탁월한 효과가 있는 수용성 키토산을 함유한 구강제제 및 그 제조방법이 개시된다. 상기 구강제제를 제조하기 위한 중간 핵심 생성물로서 탈아세틸화도가 50%인 수용성 키토산(=CTS50)을 제조하고, 제조된 탈아세틸화도가 50%인 수용성키토산을 구강청결제 원료와 배합하며, 배합된 배합물로 구강청결제를 생산한다. 상기 구강 청결제 원료로는 사포닌, 천연유래 Natural Solubilizer-K, 녹차 추출물, 프로폴리스, 자일리톨 및 효소처리스테비아로 이루어진 그룹으로부터 선택될 수 있다. By using water-soluble chitosan, which is water-soluble by acetylating chitosan, and natural ingredients beneficial to the human body as key ingredients, water-soluble chitosan is excellent for the prevention and management of oral health such as bad breath removal, periodontal care, whitening, and tartar management. An oral preparation containing the same and a method for manufacturing the same are disclosed. As an intermediate core product for manufacturing the oral preparation, water-soluble chitosan (=CTS50) with a deacetylation degree of 50% is prepared, the prepared water-soluble chitosan with a deacetylation degree of 50% is mixed with mouthwash raw materials, and the blended mixture is prepared. produces mouthwash. The mouthwash raw material may be selected from the group consisting of saponin, natural Solubilizer-K, green tea extract, propolis, xylitol, and enzyme-treated stevia.
Description
본 발명은 수용성 키토산을 함유한 구강제제 및 그 제조방법에 관한 것으로서, 더욱 상세하게는 키토산을 아세틸화하여 수용화 시킨 수용성 키토산 성분과 인체에 유익한 천연원료 성분을 핵심성분으로 활용함으로써, 구취제거, 치주관리, 미백, 치석관리 등 구강건강의 예방 및 관리에 탁월한 효과가 있는 수용성 키토산을 함유한 구강제제 및 그 제조방법에 관한 것이다. The present invention relates to an oral preparation containing water-soluble chitosan and a method for manufacturing the same. More specifically, the present invention relates to an oral preparation containing water-soluble chitosan and a method for manufacturing the same. More specifically, the present invention relates to a water-soluble chitosan component made by acetylating chitosan and making it water-soluble, and a natural raw material beneficial to the human body by using water-soluble chitosan components that are beneficial to the human body as key ingredients, thereby eliminating bad breath, It relates to an oral preparation containing water-soluble chitosan, which is excellent for preventing and managing oral health such as periodontal care, whitening, and tartar management, and a method for manufacturing the same.
치과 질환에서 가장 많이 보는 대표적인 질환의 하나로 흔히 충치라고 하며 치아우식증이라고도 한다. 치아우식증은 대부분의 선진국에서 여전히 주요 구강 건강 문제로 대두되고 있는데, 충치의 발달은 주로 Streptococcus mutans 와 Lactobacilli brevis 균주의 증식에 의해서 유발되는 것으로, 치아 우식증을 줄이기 위해 구강 세균에 항균 성분을 사용하고 있지만 일부 항균 성분이 부작용을 일으킬 수 있다.One of the most common dental diseases is commonly referred to as cavities and also called dental caries. Dental caries continues to be a major oral health problem in most developed countries. The development of cavities is mainly caused by the proliferation of Streptococcus mutans and Lactobacilli brevis strains. Although antibacterial ingredients are used against oral bacteria to reduce dental caries, Some antibacterial ingredients may cause side effects.
한편, 치주조직병이란 치아주위조직에서 발생되는 일체의 질병을 일컫는 것으로서, 치주조직병으로 인해 치아를 지지하는 조직이 점진적으로 파괴될 수 있다. On the other hand, periodontal disease refers to any disease that occurs in the tissues around the teeth, and the tissue supporting the teeth may be gradually destroyed due to periodontal disease.
이상에서 언급한 치아우식증과 치주조직병은 치아발거원인의 대부분을 차지하는 구강병으로서, 구강건강의 증진과 유지를 위하여 반드시 정복하여야 하는 양대구강병이라 할 수 있다.Dental caries and periodontal disease mentioned above are oral diseases that account for most of the causes of tooth extraction, and can be said to be two major oral diseases that must be conquered to promote and maintain oral health.
최근, 세계보건기구는 건강의 개념을 사회생활개념으로 규정하였고, 구강건강에 관한 관심이 증대되면서, 사회생활에 장애가 되는 구취의 예방과 제거에 대한 관심도 증대되었다. 이에 따라 구취의 원인과 구취제거방법에 대한 다양한 연구들이 수행되고 있다.Recently, the World Health Organization defined the concept of health as a social life concept, and as interest in oral health increased, interest in preventing and eliminating bad breath, which is an obstacle to social life, also increased. Accordingly, various studies are being conducted on the causes of bad breath and methods for eliminating bad breath.
치아우식병과 치주조직병 및 구취를 예방하고 관리하려면, 질병발생에 작용하는 숙주요인과 병원체요인 및 환경요인 중 어느 한 가지 필요요인을 없애거나 그 작용기구를 차단하여야 하는데, 병원체 요인으로는 세균과 그 독소가 주로 작용한다고 알려져 있다. 따라서, 치아우식병과 치주조직병 및 구취의 발생과 진행에 관련된 세균을 규명하고, 이러한 세균의 생장과 활동을 억제할 수 있다면, 치아우식병과 치주조직병 및 구취를 예방할 수 있다.To prevent and manage dental caries disease, periodontal disease, and bad breath, it is necessary to eliminate one of the host factors, pathogen factors, and environmental factors that play a role in disease development or block its mechanism. Pathogen factors include bacteria and It is known that the toxin mainly acts. Therefore, if the bacteria involved in the occurrence and progression of dental caries disease, periodontal disease, and bad breath can be identified and the growth and activity of these bacteria can be suppressed, dental caries disease, periodontal disease, and bad breath can be prevented.
치아우식병과 치주조직병 및 구취의 발생과 진행에 관련이 있다고 알려진 여러 세균들에 대하여, 항균력이 높으면서도 장기적으로 사용하여도 부작용이 없는 화학제나 천연추출물을 세치제나 양치액에 배합하여 사용함으로써, 구강병들을 예방하고 치료하려는 연구들이 수행되어 왔다. 특히, 천연추출물들은 화학제로 발생할 수 있는 여러 부작용들을 최소화할 수 있다는 점에서 최근 주목을 받고 있다. Against various bacteria known to be related to the occurrence and progression of dental caries disease, periodontal disease, and bad breath, the oral health is improved by using chemicals or natural extracts that have high antibacterial activity and do not cause side effects even when used over a long period of time, mixed in toothpaste or mouthwash. Research has been conducted to prevent and treat diseases. In particular, natural extracts have recently been attracting attention because they can minimize various side effects that can occur with chemical agents.
천연추출물의 한가지 예로서 키토산은 게나 가재, 새우 껍데기에 들어 있는 키틴의 아세틸아민기를 1차 아민기로 바꾸어 만들어진 다당체이다. 키토산은 인체에 무해하면서도 광범위한 균류에 항균성을 나타내어 다양한 분야에서 항미생물제제로 이용하기 위한 노력이 이루어지고 있다. 인체에 무해하면서도 항균성이 높은 키토산의 특성이 보고되면서, 구강병의 예방과 치료에 키토산을 활용할 수 있는 가능성을 제기하는 연구들이 보고된 바 있다. Chitosan, an example of a natural extract, is a polysaccharide made by changing the acetylamine group of chitin found in crab, crayfish, and shrimp shells into a primary amine group. Chitosan is harmless to the human body and has antibacterial properties against a wide range of fungi, so efforts are being made to use it as an antimicrobial agent in various fields. As the properties of chitosan, which are harmless to the human body and highly antibacterial, have been reported, studies have been reported suggesting the possibility of using chitosan for the prevention and treatment of oral diseases.
관련업계에서는 키토산의 항균 및 살균작용, 인체조직과의 친화성 등을 활용하여 구강병의 예방과 치료를 위한 제품을 개발하려는 노력들이 이루어져 왔는데, 그 중의 한 예로서, 대한민국 공개특허 제10-2000-0049546호(공개일자: 2000년 08월 05일)에는 키토산을 함유한 구강청정제가 개시되어 있는데, 상기 공개특허에서는 키토산을 구강청정제에 첨가시 일어나는 떫은 맛, 침전, 정도의 증가 등의 문제를 해결하고 기존의 구강청정제에 사용되고 있는 화학항균물질들을 대체하여 효능과 안정성 면에서 뛰어난 구강청정제를 제공하고자 하였다. In the related industry, efforts have been made to develop products for the prevention and treatment of oral diseases by utilizing chitosan's antibacterial and sterilizing effects and affinity with human tissue. One example of these is Republic of Korea Patent Publication No. 10-2000. -0049546 (publication date: August 5, 2000) discloses a mouthwash containing chitosan. The published patent addresses problems such as astringency, precipitation, and increase in severity that occur when chitosan is added to a mouthwash. The goal was to provide a mouthwash with excellent efficacy and safety by replacing the chemical antibacterial substances used in existing mouthwashes.
또한, 대한민국 등록특허 제10-0347342호(등록일자: 2002년 07월 22일)에는 수용성 고분자 키토산을 함유한 구강 청정제가 개시되어 있는데, 상기 등록특허에 따르면, 키토산 성분 중 수평균 분자량이 20∼25만인 수용성 키토산 성분이 구강내 미생물의 활성 제어에 효과가 있음에 기초하여 치아보호 및 구강 질병 예방을 위해 수평균분자량이 20∼25만인 수용성 고분자 키토산 5∼90중량%, 침강 탄산칼슘 5∼70중량%, 자일리톨 1∼20중량% 및 인산일수소칼슘 0.1∼10중량%을 포함하는 구강 청정제를 개발하였다.In addition, Republic of Korea Patent No. 10-0347342 (registration date: July 22, 2002) discloses a mouthwash containing the water-soluble polymer chitosan. According to the registered patent, the number average molecular weight of the chitosan component is 20 to 20. Based on the fact that the 250,000 water-soluble chitosan component is effective in controlling the activity of oral microorganisms, 5 to 90% by weight of water-soluble polymer chitosan with a number average molecular weight of 200,000 to 250,000 and 5 to 70% by weight of precipitated calcium carbonate are used to protect teeth and prevent oral diseases. A mouthwash containing 1 to 20% by weight of xylitol and 0.1 to 10% by weight of calcium monohydrogen phosphate was developed.
또한, 대한민국 등록특허 제10-0494747호(등록일자: 2005년 06월 01일)에는 키토산의 생체적합성, 항균활성, 면역부활작용, 생분해성 등 우수한 기능을 포함하는 항균성 구취제가 개시되어 있는데, 상기 항균성 구취제는 수용성 키토산 0.3∼0.5 중량%, 허브용액 25∼30 중량%, 젤라틴 4∼5 중량%, 용해성 전분용액 1∼2 중량% 및 나머지 물을 함유하는 필름형으로 이루어졌다.In addition, Republic of Korea Patent No. 10-0494747 (registration date: June 1, 2005) discloses an antibacterial breath freshener containing excellent features such as biocompatibility, antibacterial activity, immune activation, and biodegradability of chitosan. The antibacterial deodorant was in the form of a film containing 0.3 to 0.5% by weight of water-soluble chitosan, 25 to 30% by weight of herbal solution, 4 to 5% by weight of gelatin, 1 to 2% by weight of soluble starch solution, and the remaining water.
그런데, 위에서 언급한 선행 특허자료에 개시되어 있는 수용성 키토산관련 구강제품들의 경우에는, 키토산의 높은 구강내 항균제로서의 활용가능성에도 불구하고 최적의 항균성과 흡착력, 응집작용을 극대화할 수 있는 제조기술에 대한 충분한 연구가 이루어지지 않아서 구강제제로서의 기능을 발휘하는데 있어서 한계가 있었다. However, in the case of the water-soluble chitosan-related oral products disclosed in the prior patent materials mentioned above, despite chitosan's high usability as an oral antibacterial agent, there is no need for manufacturing technology to maximize optimal antibacterial properties, adsorption power, and coagulation. Due to insufficient research, there were limitations in its ability to function as an oral preparation.
본 발명이 해결하고자 하는 기술적 과제는, 키토산 성분 중 탈아세틸화도가 40~60% 범위인 것, 바람직하게는 탈아세틸화도가 50%인 수용성 키토산(=CTS50)을 활용하여 구취제거, 치주관리, 미백, 치석관리 등 구강건강의 예방 및 관리에 탁월한 효과가 있는 구강제제를 제공하려는 것이다.The technical problem to be solved by the present invention is to eliminate bad breath, periodontal management, The goal is to provide oral preparations that are excellent for preventing and managing oral health, such as whitening and tartar management.
또한, 본 발명이 해결하고자 하는 기술적 과제는, 다양한 기능과 용도를 가지고 있는 키틴·키토산을 수용화하는데 있어서, 가장 자연에 가까운 모습으로 수용화된 탈아세틸화도가 50%인 수용성 키토산(=CTS50)을 제공하려는 것이다. In addition, the technical problem to be solved by the present invention is to water-soluble chitin and chitosan, which have various functions and uses, by using water-soluble chitosan (=CTS50) with a deacetylation degree of 50% that is water-soluble in a form closest to nature. It is intended to provide.
전술한 바와 같은 기술적 과제를 해결하기 위해서, 본 발명은,In order to solve the technical problems described above, the present invention,
수용성 키토산을 함유한 구강제제의 제조방법으로서,As a method for manufacturing an oral preparation containing water-soluble chitosan,
(i) 상기 구강제제를 제조하기 위한 중간 핵심 생성물로서 탈아세틸화도가 50%인 수용성 키토산을 제조하는 단계(S1) - 상기 단계(S1)는,(i) Step (S1) of producing water-soluble chitosan with a degree of deacetylation of 50% as an intermediate core product for producing the oral preparation - The step (S1) includes,
(a) 탈아세틸화도 100%인 키토산으로부터 탈아세틸화도가 50%인 수용성 키토산(=CTS50)을 제조하기 위해서, 상기 탈아세틸화도 100%인 키토산을 용해하는 단계(S1-1);(a) To prepare water-soluble chitosan (=CTS50) with a deacetylation degree of 50% from chitosan with a degree of deacetylation of 100%, dissolving the chitosan with a degree of deacetylation of 100% (S1-1);
(b) 상기 단계(S1-1)를 수행한 후 용해된 액체에 무수초산과 KOH를 가하여 교반하는 단계(S1-2);(b) adding acetic anhydride and KOH to the dissolved liquid after performing the above step (S1-1) and stirring (S1-2);
(c) 상기 단계(S1-2)를 수행한 후 교반이 완료된 용액에 KOH가 희석된 용액을 넣어 1차 중화반응을 수행하는 단계(S1-3);(c) performing the first neutralization reaction by adding a diluted KOH solution to the stirred solution after performing the above step (S1-2) (S1-3);
(d) 상기 1차 중화반응을 거친 후에, 무수초산과 KOH가 용해된 증류수를 가하여 2차 중화반응을 수행하는 단계(S1-4);(d) After undergoing the first neutralization reaction, performing a second neutralization reaction by adding distilled water in which acetic anhydride and KOH are dissolved (S1-4);
(e) 상기 2차 중화반응을 거친 후에, 소정의 세척 용기(bath)에 에탄올이 용해된 증류수를 가한 다음, 상기 단계(S1-4)를 거친 용액을 가한 후 해당 용액을 응고 시키는 단계(S1-5);(e) After undergoing the secondary neutralization reaction, adding distilled water in which ethanol is dissolved in a predetermined washing vessel (bath), adding the solution that has gone through the above steps (S1-4), and then coagulating the solution (S1) -5);
(f) 상기 단계(S1-5)의 결과물로서 생긴 응고물을 상기 세척 용기에 담은 상태에서 에탄올를 가하여 세척하는 단계(S1-6);(f) washing the coagulated material resulting from the step (S1-5) in the washing container by adding ethanol (S1-6);
(g) 상기 단계(S1-6)을 수행한 후 세척 용액을 탈수하여 에탄올을 제거하는 단계(S1-7);(g) dehydrating the washing solution after performing the above step (S1-6) to remove ethanol (S1-7);
(h) 상기 단계(S1-7)를 수행하여 에탄올이 제거된 내용물을 -30℃∼-10℃ 범위의 온도로 24h 동안 냉동시키는 단계(S1-8);(h) performing the above step (S1-7) to freeze the contents from which the ethanol has been removed at a temperature ranging from -30°C to -10°C for 24 h (S1-8);
(i) 상기 단계(S1-8) 후에, 탈아세트화도(DA)가 50%에 도달할 때까지 상기 단계(S1-5) 내지 상기 단계(S1-7)을 반복적으로 수행하여 탈아세트화도(DA) 50%를 맞추는 단계(S1-9); 그리고(i) After the step (S1-8), the steps (S1-5) to (S1-7) are repeatedly performed until the deacetylation degree (DA) reaches 50% to increase the deacetylation degree (DA). DA) 50% matching step (S1-9); and
(j) 탈아세트화도(DA)가 50%에 도달하게 되면, 냉동된 키토산을 감압건조하여 플레이트(Flake) 형태로 만든 후 이를 분쇄하여 탈아세틸화도가 50%인 수용성 키토산 분말을 얻는 단계(S1-10);를 포함함 -;(j) When the degree of deacetylation (DA) reaches 50%, the frozen chitosan is dried under reduced pressure to form a plate (Flake) and then pulverized to obtain water-soluble chitosan powder with a deacetylation degree of 50% (S1) Includes -10); -;
(ⅱ) 상기 단계(S1)을 거쳐서 제조된 탈아세틸화도가 50%인 수용성키토산을 구강청결제 원료와 배합하는 단계(S2); 그리고(ii) mixing water-soluble chitosan with a degree of deacetylation of 50% prepared through the above step (S1) with mouthwash raw materials (S2); and
(ⅲ) 상기 단계(S2)에서 배합된 배합물로 구강청결제를 생산하는 단계(S3);를 포함하는 수용성 키토산을 함유한 구강제제의 제조방법을 제공한다.(iii) a step (S3) of producing an mouthwash using the mixture prepared in step (S2); providing a method for producing an oral preparation containing water-soluble chitosan, including a step (S3).
상기 단계(S2)는, The step (S2) is,
1L의 물 용매에 1g~10g의 탈아세틸화도가 50%인 수용성 키토산을 용질로써 녹여 미네랄 칼슘이 전체 배합물의 0.10중량%~1.0중량%가 되도록 하는 단계(S2-1);Step (S2-1) of dissolving 1g to 10g of water-soluble chitosan with a deacetylation degree of 50% in 1L of water solvent as a solute so that the mineral calcium is 0.10% to 1.0% by weight of the total mixture;
탈아세틸화도가 50%인 수용성 키토산이 용출된 수용액의 항균성이 향상되도록 1~3일 동안 두어 침전물을 침전시켜 안정화 시키는 단계(S2-2); 그리고A step of stabilizing the precipitate by allowing it to precipitate for 1 to 3 days to improve the antibacterial properties of the aqueous solution in which water-soluble chitosan with a degree of deacetylation of 50% is eluted (S2-2); and
안정화된 수용액의 침전물을 제거하여 깨끗한 수용액을 얻는 단계(S2-3);를 포함하는 것을 특징으로 한다.It is characterized in that it includes a step (S2-3) of removing the precipitate of the stabilized aqueous solution to obtain a clean aqueous solution.
상기 단계(S2-3)를 거치면서 얻어진 깨끗한 수용액에 상기 구강청결제 원료를 배합하되, 상기 구강청결제 원료는, 전체 배합물의 중량을 100중량%로 했을 때, 사포닌 4.0중량%, 프로폴리스 0.5중량%, 자일리톨 2.8중량%를 안정화된 수용액과 배합하는 것을 특징으로 한다.The mouthwash raw materials are mixed with the clean aqueous solution obtained through the above step (S2-3), wherein the mouthwash raw materials include 4.0% by weight of saponin and 0.5% by weight of propolis, when the weight of the total mixture is 100% by weight. , characterized in that 2.8% by weight of xylitol is blended with a stabilized aqueous solution.
이상에서 살펴본 바와 같이, 본 발명에 따른 탈아세틸화도가 50%인 수용성 키토산(=CTS50)을 기초로 제조된 구강제제는, 구강세균에 대한 항균성, 구취제거 성능이 우수하여 구강제제로의 응용에 있어 뛰어난 적합성을 나타낸다. 또한, 여러 가지 우수한 물리적인 특성으로 인해 기존 구강제제의 여러 가지 문제점을 해결함과 동시에 제약산업에서의 활용 가능성이 확대될 것이다. As seen above, the oral preparation prepared based on water-soluble chitosan (=CTS50) with a deacetylation degree of 50% according to the present invention has excellent antibacterial properties against oral bacteria and bad breath removal performance, making it suitable for application as an oral preparation. It shows excellent suitability. In addition, due to its various excellent physical properties, it will solve various problems of existing oral preparations and expand its potential for use in the pharmaceutical industry.
도 1은 본 발명에 따른 수용성 키토산을 함유한 구강제제의 제조 공정도.Figure 1 is a manufacturing process diagram of an oral preparation containing water-soluble chitosan according to the present invention.
이하, 본 발명에 따른 수용성 키토산을 함유한 구강제제의 제조방법에 대해 상세하게 설명한다. Hereinafter, the method for producing an oral preparation containing water-soluble chitosan according to the present invention will be described in detail.
본 발명에서는 출발재료로서 다양한 분자량을 갖는 탈아세틸화도 100%인 키토산을 사용하고, 키토산 성분중 탈아세틸화도가 40∼60% 범위인 것이 수용성을 나타내는 것에 기초하여 바람직하게는 탈아세틸화도가 50%인 수용성 키토산(이하, "CTS50" 이라 함)을 구강제제를 제조하기 위한 중간 핵심 생성물로 제조하는 것이다.In the present invention, chitosan with various molecular weights and a degree of deacetylation of 100% is used as a starting material, and based on the fact that chitosan components with a degree of deacetylation in the range of 40 to 60% exhibit water solubility, preferably a degree of deacetylation of 50%. Phosphorus-soluble chitosan (hereinafter referred to as “CTS50”) is manufactured as an intermediate core product for manufacturing oral preparations.
본 출원인겸 발명자는, 본 발명에 따른 수용성 키토산을 함유한 구강제제의 제조방법에 대해 설명하기에 앞서서, 대한민국 공개특허 제10-2010-0087418호(공개일자: 2010년 08월 05일/ 출원인: 주식회사영키팜)에 개시된 수용성 키토산 제조법의 공동 개발자로 참여한 바 있으며 상기 공개특허 제10-2010-0087418호에 개시되었던 수용성 키토산 제조과정중 일부를 기초하여 이를 개선 및 발전시켜서 금번 본 발명을 완성하게 되었음을 밝히는 바이다.Before explaining the manufacturing method of the oral preparation containing water-soluble chitosan according to the present invention, the present applicant and inventor, Republic of Korea Patent Publication No. 10-2010-0087418 (publication date: August 5, 2010 / Applicant: We have participated as a co-developer of the water-soluble chitosan manufacturing method disclosed by Youngkipharm Co., Ltd., and have completed the present invention by improving and developing it based on part of the water-soluble chitosan manufacturing process disclosed in Patent Publication No. 10-2010-0087418. This is to reveal.
본 발명에 따른 수용성 키토산을 함유한 구강제제의 제조방법에서 첫번째 단계는 상기 구강제제를 제조하기 위한 중간 핵심 생성물로서 탈아세틸화도가 50%인 수용성 키토산을 제조하는 것이다(=단계 S1). The first step in the method for producing an oral preparation containing water-soluble chitosan according to the present invention is to prepare water-soluble chitosan with a degree of deacetylation of 50% as an intermediate core product for producing the oral preparation (=step S1).
상기 단계(S1)은 여러가지의 과정을 거치게 되는데, 먼저 탈아세틸화도 100%인 키토산으로부터 탈아세틸화도가 40∼60% 범위인 키토산, 바람직하게는 CTS50을 제조하기 위해서, 점도 8~100CPS, 탈아세틸화도 100%인 키토산 20g을 아세트산 20㎖와 증류수 2ℓ의 혼합액에 용해한다. 이때, 온도는 50~60℃를 유지한다(=단계 S1-1). The step (S1) goes through various processes. First, in order to produce chitosan with a deacetylation degree of 40 to 60%, preferably CTS50, from chitosan with a deacetylation degree of 100%, a viscosity of 8 to 100 CPS, deacetylation Dissolve 20g of 100% chitosan in a mixture of 20ml of acetic acid and 2l of distilled water. At this time, the temperature is maintained at 50-60°C (=step S1-1).
다음에는, 용해된 액체에 무수초산 6㎖를 가하여 약 1시간 동안 교반한 후, KOH 12g을 물 100㎖에 녹여 가한 다음 다시 무수초산 2㎖를 가하여 20분 교반한 후 KOH 6g을 물 50㎖에 녹여 1시간 교반한다(=단계 S1-2). 상기 단계(S1-2)에 있어서, 무수초산의 양은 키토산 무게의 20~40%가 바람직하다. 본 발명에서 탈아세틸화도는 무수초산의 양과 반응시간에 가장 민감하였다.Next, 6 ml of acetic anhydride was added to the dissolved liquid and stirred for about 1 hour. Then, 12 g of KOH was dissolved in 100 ml of water, and then 2 ml of acetic anhydride was added again and stirred for 20 minutes. Then, 6 g of KOH was added to 50 ml of water. Dissolve and stir for 1 hour (=step S1-2). In the step (S1-2), the amount of acetic anhydride is preferably 20 to 40% of the weight of chitosan. In the present invention, the degree of deacetylation was most sensitive to the amount of acetic anhydride and reaction time.
다음에는, 교반이 완료된 용액에 1g의 KOH가 희석된 용액 20㎖을 넣어 36℃의 용기(bath)에서 pH4가 될 때까지 1차 중화반응을 거친다(=단계 S1-3). Next, 20 ml of a diluted solution of 1 g of KOH is added to the stirred solution and subjected to a primary neutralization reaction until pH reaches 4 in a bath at 36°C (=step S1-3).
1차 중화반응을 거친 후에는, 무수초산을 7㎖와 KOH 0.3g이 용해된 증류수 1ℓ를 가한 후 36℃의 용기(bath)에서 pH8이 될 때까지 2시간 동안 2차 중화반응을 거친다(=단계 S1-4). After going through the first neutralization reaction, add 7 ml of acetic anhydride and 1 liter of distilled water with 0.3 g of KOH dissolved in it, and then go through the second neutralization reaction in a bath at 36°C for 2 hours until pH reaches 8 (= Step S1-4).
2차 중화반응을 거친 후에는, 별도의 세척 용기(bath)에 에탄올 500mg이 용해된 증류수 1ℓ를 가한 후, 상기 단계(S1-4)를 거친 용액을 가한 다음 해당 용액을 응고 시킨다(=단계 S1-5). After the secondary neutralization reaction, 1 liter of distilled water with 500 mg of ethanol dissolved in it is added to a separate washing vessel (bath), then the solution passed through the above steps (S1-4) is added, and the solution is solidified (=step S1) -5).
다음에는, 상기 세척 용기에 상기 단계(S1-5)의 결과물로서 생긴 응고물을 담은 상태에서 에탄올 1ℓ를 가하여 60분 정도 담가 세척한다(=단계 S1-6). Next, 1 liter of ethanol is added to the washing container containing the coagulated material resulting from step (S1-5), soaked for about 60 minutes, and washed (=step S1-6).
상기 단계(S1-6)을 수행한 후 세척 용액을 탈수하여 에탄올을 제거한다(=단계 S1-7). After performing the above step (S1-6), the washing solution is dehydrated to remove ethanol (=step S1-7).
상기 단계(S1-7)를 수행하여 에탄올이 제거된 내용물을 선반에 펼쳐서 -30℃∼-10℃ 범위의 온도로 24h 냉동시킨다(=단계 S1-8). The content from which the ethanol has been removed by performing the above step (S1-7) is spread on a shelf and frozen for 24 hours at a temperature in the range of -30°C to -10°C (=step S1-8).
상기 단계(S1-8) 후에는, 탈아세트화도(DA)가 40~60% 범위에 있는지를 체크하고, 목표치에 도달할 때까지 상기 단계(S1-5) 내지 상기 단계(S1-7)을 반복적으로 수행하여 탈아세트화도(DA)를 맞춘다(=단계 S1-9). After the step (S1-8), check whether the degree of deacetylation (DA) is in the range of 40 to 60%, and repeat the steps (S1-5) to (S1-7) until the target value is reached. Perform the process repeatedly to adjust the degree of deacetylation (DA) (=step S1-9).
탈아세트화도(DA)가 목표치인 40~60% 범위에 도달하게 되면, 냉동된 키토산을 감압건조하여 플레이트(Flake) 형태로 만든 후 이를 분쇄하여 탈아세틸화도가 50%인 수용성 키토산(=CTS50) 분말을 얻는다(=단계 S1-10). 이렇게 얻어진 분말은 용해하여 겔이나 액상 형태로도 사용이 가능하다.When the degree of deacetylation (DA) reaches the target range of 40 to 60%, the frozen chitosan is dried under reduced pressure to form flakes and then pulverized to produce water-soluble chitosan with a degree of deacetylation of 50% (=CTS50). Obtain powder (=step S1-10). The powder obtained in this way can be dissolved and used in gel or liquid form.
본 발명에 따르면, 전술한 바와 같은 과정을 거쳐서 제조한 탈아세트화도(DA) 40~60%, 바람직하게는 CTS50을 이용하여 구강제제를 얻는다. 본 발명은 치주질환 예방과 개선에 도움이 되는 CTS50 수용성 키토산 성분과 천연원료를 활용한 치약, 정체형 가글, 구강가글(=청결제) 등 천연 구강제제를 제공하고자 한다. According to the present invention, an oral preparation is obtained using a deacetylation degree (DA) of 40 to 60%, preferably CTS50, prepared through the process described above. The present invention seeks to provide natural oral preparations such as toothpaste, static gargle, and oral gargle (=cleanser) using CTS50 water-soluble chitosan ingredient and natural raw materials that are helpful in preventing and improving periodontal disease.
주지하는 바와 같이, 구강제제는 치약, 구강청결제 등 다양한 종류들이 있으며, 이들의 사용 목적은 구취제거, 치주관리, 미백, 치석관리 등 구강건강의 예방 및 관리에 도움을 주는 것이다. 그러나, 이러한 구강제제의 제조 시 색소, 향료, 살균소독제(알코올), 치석용해제, 유화제, 보존제 등 인체에 유해한 물질들이 함유되어 제조되기 때문에 구강 건조증, 치아 반점 생성, 다양한 전신질환 위험 노츨 등의 부작용을 야기하게 된다. As you know, there are various types of oral preparations, such as toothpaste and mouthwash, and the purpose of their use is to help prevent and manage oral health such as bad breath removal, periodontal care, whitening, and tartar management. However, when manufacturing these oral preparations, they contain substances harmful to the human body, such as pigments, fragrances, disinfectants (alcohol), tartar dissolvers, emulsifiers, and preservatives, so they can cause side effects such as dry mouth, spots on teeth, and risk of various systemic diseases. causes.
따라서, 본 발명은 인체에 유해한 화학조성물을 첨가하지 않은 천연 기능성 성분들로 만든 안전한 가글형 구강제제 또는 사용 및 휴대가 간편한 치아플라그 착색용 정제형 구강제제를 제공하려는 것이다. Therefore, the present invention is intended to provide a safe gargle-type oral preparation or a tablet-type oral preparation for tooth plaque staining that is easy to use and carry, made from natural functional ingredients without adding chemical compositions harmful to the human body.
먼저, 구강관리를 위한 가글형 구강제제를 제조하기 위해서, 본 발명은, 앞서 설명한 CTS50 제조단계를 거쳐서 제조된 수용성키토산을 구강청결제 원료와 배합하는 단계(S2); 및 상기 단계(S2)에서 배합된 배합물로 구강청결제를 생산하는 단계(S3)를 포함한다. First, in order to manufacture a gargle-type oral preparation for oral care, the present invention includes the step of mixing water-soluble chitosan prepared through the CTS50 manufacturing step described above with mouthwash raw materials (S2); and a step (S3) of producing a mouthwash using the mixture prepared in step (S2).
상기 단계(S2)에서는, 앞서 설명한 바와 같이 탈아세틸화도 100%인 키토산으로부터 탈아세틸화도가 50%인 키토산 CTS50을 제조하는 단계(S1)를 거쳐서 제조된 CTS50을 전체 배합물 중량 대비 0.10중량%~1.0중량% 함유시키고, 나머지의 구강 청결제 원료를 배합하게 되는데, 이때 구강 청결제 원료로는 사포닌, 천연유래 Natural Solubilizer-K, 녹차 추출물, 프로폴리스, 자일리톨, 효소처리스테비아를 포함한다.In the step (S2), as described above, CTS50 prepared through the step (S1) of producing chitosan CTS50 with a 50% deacetylation degree from chitosan with a 100% deacetylation degree is added to 0.10% by weight to 1.0% by weight based on the total weight of the mixture. % by weight, and the remaining mouthwash raw materials are mixed. At this time, the mouthwash raw materials include saponin, naturally derived Natural Solubilizer-K, green tea extract, propolis, xylitol, and enzyme-treated stevia.
상기 단계(S2)의 구체적인 실시 예로서, 1L의 물 용매에 1g~10g의 CTS50을 용질로써 녹여, 미네랄 칼슘이 전체 배합물의 0.10중량%~1.0중량%가 되도록 하고(=단계 S2-1), CTS50이 용출된 수용액의 항균성이 향상되도록 1~3일 동안 두어 침전물을 침전시켜 안정화 시킨다(=단계 S2-2). 다음에는, 안정화된 수용액의 침전물을 제거한다(=단계 S2-3). 즉, 안정화된 수용액의 침전물을 제거하여 깨끗한 수용액을 얻는다. As a specific example of the step (S2), 1g to 10g of CTS50 is dissolved as a solute in 1L of water solvent so that the mineral calcium is 0.10% to 1.0% by weight of the total mixture (=step S2-1), To improve the antibacterial properties of the aqueous solution in which CTS50 is eluted, the solution is left for 1 to 3 days to precipitate and stabilize the precipitate (=step S2-2). Next, the precipitate of the stabilized aqueous solution is removed (=step S2-3). That is, the precipitate in the stabilized aqueous solution is removed to obtain a clean aqueous solution.
상기 단계(S2-3)를 거치면서 얻어진 깨끗한 수용액에 앞서 언급한 구강청결제 원료를 배합한다. 구체적으로는, 구강청결제 원료로서, 전체 배합물의 중량을 100중량%로 했을 때, 사포닌 4.0중량%, 프로폴리스 0.5중량%, 자일리톨 2.8중량%를 안정화된 수용액과 배합한다. 특히, 사포닌은 천연 유화제로서 사용이 가능하며, 4.0중량% 이상 포함시 유화가 잘 이루어짐은 확인하였다. The previously mentioned mouthwash raw materials are mixed with the clean aqueous solution obtained through the above steps (S2-3). Specifically, as a raw material for mouthwash, when the total weight of the mixture is 100% by weight, 4.0% by weight of saponin, 0.5% by weight of propolis, and 2.8% by weight of xylitol are mixed with a stabilized aqueous solution. In particular, saponin can be used as a natural emulsifier, and it was confirmed that emulsification is achieved well when it is included at 4.0% by weight or more.
한편, 기존의 구강 청결제에는 구강 내 세균을 억제하기 위하여, 여러가지 인체에 유해한 영향을 미치는 합성화학물질을 이용하여 제조되기 때문에, 구강 청결제를 뱉은 후에도 구강 내에 화학성분이 잔류하게 되어, 침을 삼킬 때 잔류하는 화학성분을 함께 삼킬 가능성이 있다는 문제점이 존재하였다. 구강청결제의 원료로 사용되는 불소는 충치를 예방하기 위해 사용되는데, 하지만 불소를 한번에 많이 먹으면 위장 장애, 구토 등이 생길 수 있고 장기간 섭취했을 때 치아에 하얀 반점이 생기는 반상치가 생기기도 하며, 특히, 어린아이들의 경우 구강청결제를 자주 삼키고 구강 내를 잘 헹구어 내지 못하므로 불소로 인한 위험성이 더 크다.Meanwhile, existing mouthwashes are manufactured using synthetic chemicals that have various harmful effects on the human body in order to suppress bacteria in the oral cavity, so chemical components remain in the oral cavity even after spitting out the mouthwash, causing irritation when swallowing saliva. There was a problem that there was a possibility of swallowing the remaining chemical ingredients together. Fluoride, which is used as a raw material for mouthwash, is used to prevent cavities. However, if you consume a lot of fluoride at once, it can cause gastrointestinal problems and vomiting, and if consumed for a long period of time, it can cause white spots on the teeth, especially chipped teeth. Young children are at greater risk from fluoride because they frequently swallow mouthwash and are unable to rinse their mouths well.
이에 비해서, 본 발명에 따른 구강청결제의 제조방법에 의해 제조된 구강청결제는 항균효과가 있는 CTS50을 포함함으로써, 구강청결제 원료로 사용되는 불소를 기존의 구강청결제보다 적게 사용할 수 있다. In comparison, the mouthwash manufactured by the method of manufacturing the mouthwash according to the present invention contains CTS50, which has an antibacterial effect, so that less fluoride, which is used as a raw material for the mouthwash, can be used than in existing mouthwashes.
한편, 기존의 구강청결제의 원료로서 유화제로 많이 쓰이는 오일류나 각종 화학 공정을 통해 얻어진 각종 추출물 등은 원료 제조과정에서 사용되는 PEG 성분이 발암물질로서 피부 침투력이 우수하여 암의 발생이나 알레르기 반응, 접촉성 피부염 및 신경계의 독성을 유발하는 문제점이 있으나, 유화제(가용화제)로서의 효과가 뛰어나 일반적으로 널리 사용되고 있다. 세계적인 구강청결제 제조사에서 시판하고 있는 제품 등에는 이러한 PEG 이외에도 순간적인 사용감의 만족성을 제공하기 위하여 청정, 살균 및 항균 등을 위해 알코올이 다량 첨가되어 있어 구강 건조증을 유발하고 시간의 경과에 따라 구취를 발생하며 구내염과 구강암 등을 유발한다는 연구들이 발표되고 있다. On the other hand, oils, which are widely used as emulsifiers as raw materials for existing mouthwashes, and various extracts obtained through various chemical processes, contain PEG components used in the raw material manufacturing process, which are carcinogens and have excellent skin penetration, causing cancer, allergic reactions, and contact. Although it has the problem of causing sexual dermatitis and nervous system toxicity, it is widely used because of its excellent effect as an emulsifier (solubilizer). In addition to PEG, products sold by global mouthwash manufacturers contain a large amount of alcohol for cleaning, sterilization, and antibacterial purposes in order to provide instantaneous satisfaction, causing dry mouth and bad breath over time. Studies have shown that it causes stomatitis and oral cancer.
이에 비해서 본 발명의 CTS50과 고함량의 사포닌을 함유한 구강청결제는 기존에 사용되어지는 오일류, 각종 추출물 PEG 성분 등을 완전 제거하여 제조함으로서 사용자들이 보다 안전하게 구강청결제를 사용할 수 있으며, 특히 구강청결제를 자주 삼키고 구강청결제를 잘 헹구어 내지 못하는 어린아이들이나 임산부, 노인들이 안전하게 사용할 수 있다.In contrast, the mouthwash containing CTS50 and a high content of saponin of the present invention is manufactured by completely removing previously used oils, various extracts and PEG components, so users can use the mouthwash more safely, especially the mouthwash. It can be safely used by young children, pregnant women, and the elderly who swallow frequently and are unable to rinse off mouthwash properly.
또한, 본 발명의 실시예에 따른 CTS50을 포함하는 구강청결제의 제조방법에 의해 제조된 구강청결제는 항균 물질로, 미네랄 칼슘을 포함함으로써, 다른 항균성 물질을 포함하지 않아도 그 자체로 우수한 항균성을 가져 사용자가 기존의 구강청결제보다 안전하게 사용할 수 있다.In addition, the mouthwash manufactured by the method of manufacturing a mouthwash containing CTS50 according to an embodiment of the present invention is an antibacterial material and contains mineral calcium, so it has excellent antibacterial properties on its own even without containing other antibacterial materials. It is safer to use than existing mouthwashes.
또한, 본 발명의 실시예에 따른 CTS50을 포함하는 구강청결제의 제조방법에 의해 제조된 구강청결제에는, 프로폴리스 추출물이 첨가되어, 프로폴리스 향을 가질 수 있으며, 세균의 침투를 예방하고, 박멸하는 기능을 가질 수 있다. In addition, the mouthwash manufactured by the method of manufacturing a mouthwash containing CTS50 according to an embodiment of the present invention may have a propolis scent by adding propolis extract, and may prevent the penetration and eradication of bacteria. It can have functions.
또한, 본 발명의 CTS50을 포함하는 구강청결제의 제조방법에 의해 제조된 구강청결제에는, 자일리톨이 첨가되어, 단맛을 낼 수 있으며, 충치의 원인균인 스트렙토코커스 뮤탄스균(Streptococcus mutants)의 생성을 억제할 수 있다. In addition, xylitol is added to the mouthwash manufactured by the method of manufacturing a mouthwash containing CTS50 of the present invention, which can give it a sweet taste and inhibit the production of Streptococcus mutants, which are the causative bacteria of cavities. You can.
상기 단계(S2)에서 배합된 배합물로 구강청결제를 생산하는 단계(S3)에서, CTS50을 포함하는 구강청결제는 별도로 제작된 통에 담겨 포장될 수 있다. In the step (S3) of producing a mouthwash using the mixture mixed in the step (S2), the mouthwash containing CTS50 may be packaged in a separately manufactured container.
이상에서 언급한 바와 같이, 본 발명에서 제안하고 있는 탈아세틸화도가 50%인 수용성키토산(CTS50)을 포함하는 구강청결제는, 구강청결제에 알코올이나 다른 항균물질들을 포함하지 않아도 그 자체로서 우수한 항균력 및 구취억제 등의 효과를 가질 수 있다. 또한, 임상적으로 효과가 입증된 수용성키토산(CTS50)을 이용하여 제조된 구강청결제는 다른 항균 조성물들을 이용하는 경우에 비해 적은 양만으로도 구강세균에 대한 항균성 및 구취억제를 확보할 수 있다.As mentioned above, the mouthwash containing water-soluble chitosan (CTS50) with a deacetylation degree of 50% proposed in the present invention has excellent antibacterial activity and It can have effects such as suppressing bad breath. In addition, mouthwash manufactured using water-soluble chitosan (CTS50), which has been clinically proven to be effective, can secure antibacterial properties against oral bacteria and suppress bad breath with a small amount compared to using other antibacterial compositions.
뿐만 아니라, 본 발명에서 제안하고 있는 수용성키토산(CTS50)을 포함하는 구강청결제의 제조방법에 따르면, 수용성키토산(CTS50)은 구강관리용 형태로 사용되는 일반적인 구강청결제 형태로 구현되므로, 구강청결제에 포함된 수용성키토산(CTS50)에 의한 항균 효과가 지속적으로 유지되며, 치주질환이나 구취유발의 원인균에 대한 항균작용은 물론, 치주질환 및 구내염 등 구강내 염증도 완화 및 예방할 수 있다. In addition, according to the method for manufacturing a mouthwash containing water-soluble chitosan (CTS50) proposed in the present invention, water-soluble chitosan (CTS50) is implemented in the form of a general mouthwash used for oral care and is therefore included in the mouthwash. The antibacterial effect of water-soluble chitosan (CTS50) is maintained continuously, and not only has an antibacterial effect against bacteria that cause periodontal disease and bad breath, but it can also alleviate and prevent oral inflammation such as periodontal disease and stomatitis.
게다가, 수용성키토산(CTS50)을 이용하여 구강청결제를 제조함으로써, 항염 및 치주질환이나 구취유발의 원인균을 억제하고 효율적인 구강관리가 이루어질 수 있어 일반적인 구강청결제에 사용되는 인체에 유해한 화학약품의 사용을 원천적으로 예방할 수 있다.In addition, by manufacturing mouthwash using water-soluble chitosan (CTS50), effective oral care can be achieved by suppressing anti-inflammatory and bacteria that cause periodontal disease or bad breath, eliminating the use of chemicals harmful to the human body that are used in general mouthwash. It can be prevented.
본 발명에 따라 제조된 CTS50의 항균작용에 대한 실험결과 및 고찰Experimental results and consideration of the antibacterial effect of CTS50 prepared according to the present invention
하기에서는 구강세균에 대한 키토산(CTS50)의 항균작용을 그림 1 내지 그림 3에 그래프로 나타내었다. In the following, the antibacterial activity of chitosan (CTS50) against oral bacteria is shown graphically in Figures 1 to 3.
그림 1. CTS50 키토산 및 클로로헥시딘에 대한 Streptococcus mutans의 5분 노출 후 생장곡선Figure 1. Growth curve of Streptococcus mutans after 5 minutes exposure to CTS50 chitosan and chlorhexidine.
그림 2. CTS50 키토산 및 클로로헥시딘에 대한 Phopyromonas gingivalis의 5분 노출 후 생장곡선Figure 2. Growth curve of Phopyromonas gingivalis after 5 min exposure to CTS50 chitosan and chlorhexidine.
그림 3. CTS50 키토산 및 클로로헥시딘에 대한 Fusobacterium nucleatum의 5분 노출 후 생장곡선Figure 3. Growth curve of Fusobacterium nucleatum after 5 minutes exposure to CTS50 chitosan and chlorhexidine.
상기 그림 1 내지 3에서 그래프로 나타난 바와 같이, 본 발명의 수용성 키토산(CTS50)은 시험된 대부분의 박태리아 성장을 크게 억제하였다. 또한, 키토산의 최소저해농도(MIC)값은 P.aeruginosa(.25%)의 경우를 제외하고는 Gram negative bacteria에 대해 0.06%이하였다.As shown graphically in Figures 1 to 3 above, the water-soluble chitosan (CTS50) of the present invention significantly inhibited the growth of most bacteria tested. In addition, the minimum inhibitory concentration (MIC) value of chitosan was less than 0.06% against Gram negative bacteria, except for P. aeruginosa (.25%).
참고로, 키토산(탈아세틸화도 : 82%)은 자광(주)의 것을 사용하였고, 항미생물 활성을 측정하기 위해 사용된 미생물은 KCTC(Collection of Type Culture)와 ATCC(American Type Culture Collection)사의 것을 사용하였다.For reference, chitosan (degree of deacetylation: 82%) was from Jakwang Co., Ltd., and the microorganisms used to measure antimicrobial activity were from KCTC (Collection of Type Culture) and ATCC (American Type Culture Collection). used.
본 발명의 수용성 키토산(CTS50)은 다양한 점도를 가진 키토산을 이용하여 제조할 수 있으며, 무수초산의 양이 많아질수록 탈아세틸화도(=DA)가 낮아졌고, 또한 반응시간이 길수록 DA가 낮아졌다. The water-soluble chitosan (CTS50) of the present invention can be manufactured using chitosan with various viscosities. As the amount of acetic anhydride increased, the degree of deacetylation (=DA) decreased, and as the reaction time increased, DA decreased.
본 발명에서 DA가 낮을수록 pH에 대한 안정성이 높아지는 반면, 너무 낮은 DA를 가지면 불용분이 증가하였다(DA 30%이하). 또한, DA가 높을수록(60%이상일 때) 떫은 맛을 점점 나타내었고, pH에 대한 안정성도 낮아졌다.In the present invention, the lower the DA, the higher the stability against pH, whereas if the DA is too low, the insoluble matter increases (DA 30% or less). In addition, the higher the DA (above 60%), the more astringent the taste was, and the lower the stability to pH.
본 발명에서의 pH의 안정성은 키틴과 키토산의 비율이 비슷한 경우, 수소결합의 약화에 기인하며, 또한 이것이 수용화의 원인이라 할 수 있다. The stability of pH in the present invention is due to the weakening of hydrogen bonds when the ratio of chitin and chitosan is similar, and this can also be said to be the cause of water solubilization.
CTS50는 키토산을 다시 아세틸화하여 아세틸정도를 50% 정도로 한 것으로, 다시 말해서 아세틸화가 약 50%된 키토산이다. 따라서, CTS50은 키틴과 키토산의 기능을 모두 가지고 있다는 장점이 있으며, 떫은 맛이 전혀 없는 특징을 가진다. 또한 이것은 수용성이므로 사용이 용이하며, 보통의 키토산보다 pH에 민감하지 않아 기타 약제와 혼용 시 변질의 우려가 낮다.CTS50 is chitosan that has been acetylated again to reduce the acetylation level to about 50%. In other words, it is chitosan that has been acetylated to about 50%. Therefore, CTS50 has the advantage of having the functions of both chitin and chitosan, and has no astringent taste at all. In addition, it is easy to use because it is water-soluble, and is less sensitive to pH than ordinary chitosan, so there is less risk of deterioration when mixed with other drugs.
S1, S1-1∼S1-10, S2, S3 : 단계S1, S1-1∼S1-10, S2, S3: Steps
Claims (10)
(i) 상기 구강제제를 제조하기 위한 중간 핵심 생성물로서 탈아세틸화도가 50%인 수용성 키토산을 제조하는 단계(S1) - 상기 단계(S1)는,
(a) 탈아세틸화도 100%인 키토산으로부터 탈아세틸화도가 50%인 수용성 키토산(=CTS50)을 제조하기 위해서, 상기 탈아세틸화도 100%인 키토산을 용해하는 단계(S1-1);
(b) 상기 단계(S1-1)를 수행한 후 용해된 액체에 무수초산과 KOH를 가하여 교반하는 단계(S1-2);
(c) 상기 단계(S1-2)를 수행한 후 교반이 완료된 용액에 KOH가 희석된 용액을 넣어 1차 중화반응을 수행하는 단계(S1-3);
(d) 상기 1차 중화반응을 거친 후에, 무수초산과 KOH가 용해된 증류수를 가하여 2차 중화반응을 수행하는 단계(S1-4);
(e) 상기 2차 중화반응을 거친 후에, 소정의 세척 용기(bath)에 에탄올이 용해된 증류수를 가한 다음, 상기 단계(S1-4)를 거친 용액을 가한 후 해당 용액을 응고 시키는 단계(S1-5);
(f) 상기 단계(S1-5)의 결과물로서 생긴 응고물을 상기 세척 용기에 담은 상태에서 에탄올를 가하여 세척하는 단계(S1-6);
(g) 상기 단계(S1-6)을 수행한 후 세척 용액을 탈수하여 에탄올을 제거하는 단계(S1-7);
(h) 상기 단계(S1-7)를 수행하여 에탄올이 제거된 내용물을 -30℃∼-10℃ 범위의 온도로 24h 동안 냉동시키는 단계(S1-8);
(i) 상기 단계(S1-8) 후에, 탈아세트화도(DA)가 50%에 도달할 때까지 상기 단계(S1-5) 내지 상기 단계(S1-7)을 반복적으로 수행하여 탈아세트화도(DA) 50%를 맞추는 단계(S1-9); 그리고
(j) 탈아세트화도(DA)가 50%에 도달하게 되면, 냉동된 키토산을 감압건조하여 플레이트(Flake) 형태로 만든 후 이를 분쇄하여 탈아세틸화도가 50%인 수용성 키토산 분말을 얻는 단계(S1-10);를 포함함 -;
(ⅱ) 상기 단계(S1)을 거쳐서 제조된 탈아세틸화도가 50%인 수용성키토산을 구강청결제 원료와 배합하는 단계(S2) - 상기 단계(S2)는,
1L의 물 용매에 1g~10g의 탈아세틸화도가 50%인 수용성 키토산을 용질로써 녹여 칼슘이 전체 배합물의 0.10중량%~1.0중량%가 되도록 하는 단계(S2-1);
탈아세틸화도가 50%인 수용성 키토산이 용출된 수용액의 항균성이 향상되도록 1~3일 동안 두어 침전물을 침전시켜 안정화 시키는 단계(S2-2); 및
안정화된 수용액의 침전물을 제거하여 깨끗한 수용액을 얻는 단계(S2-3);를 포함함 -; 그리고
(ⅲ) 상기 단계(S2)에서 배합된 배합물로 구강청결제를 생산하는 단계(S3);
를 포함하는 수용성 키토산을 함유한 구강제제의 제조방법.
As a method for manufacturing an oral preparation containing water-soluble chitosan,
(i) Step (S1) of producing water-soluble chitosan with a degree of deacetylation of 50% as an intermediate core product for producing the oral preparation - The step (S1) includes,
(a) To prepare water-soluble chitosan (=CTS50) with a deacetylation degree of 50% from chitosan with a degree of deacetylation of 100%, dissolving the chitosan with a degree of deacetylation of 100% (S1-1);
(b) adding acetic anhydride and KOH to the dissolved liquid after performing the above step (S1-1) and stirring (S1-2);
(c) performing the first neutralization reaction by adding a diluted KOH solution to the stirred solution after performing the above step (S1-2) (S1-3);
(d) After undergoing the first neutralization reaction, performing a second neutralization reaction by adding distilled water in which acetic anhydride and KOH are dissolved (S1-4);
(e) After undergoing the secondary neutralization reaction, adding distilled water in which ethanol is dissolved in a predetermined washing vessel (bath), adding the solution that has gone through the above steps (S1-4), and then coagulating the solution (S1) -5);
(f) washing the coagulated material resulting from the step (S1-5) in the washing container by adding ethanol (S1-6);
(g) dehydrating the washing solution after performing the above step (S1-6) to remove ethanol (S1-7);
(h) performing the above step (S1-7) and freezing the contents from which the ethanol has been removed at a temperature ranging from -30°C to -10°C for 24 h (S1-8);
(i) After the step (S1-8), the steps (S1-5) to (S1-7) are repeatedly performed until the deacetylation degree (DA) reaches 50% to increase the deacetylation degree (DA). DA) 50% matching step (S1-9); and
(j) When the degree of deacetylation (DA) reaches 50%, the frozen chitosan is dried under reduced pressure to form a plate (Flake) and then pulverized to obtain water-soluble chitosan powder with a deacetylation degree of 50% (S1) Includes -10); -;
(ii) Step (S2) of mixing water-soluble chitosan with a degree of deacetylation of 50% prepared through step (S1) with mouthwash raw materials - In step (S2),
Step (S2-1) of dissolving 1g to 10g of water-soluble chitosan with a deacetylation degree of 50% in 1L of water solvent as a solute so that calcium is 0.10% to 1.0% by weight of the total mixture;
A step of stabilizing the precipitate by allowing it to precipitate for 1 to 3 days to improve the antibacterial properties of the aqueous solution in which water-soluble chitosan with a degree of deacetylation of 50% is eluted (S2-2); and
Including a step (S2-3) of removing precipitates from the stabilized aqueous solution to obtain a clean aqueous solution; and
(iii) a step (S3) of producing a mouthwash using the mixture prepared in step (S2);
A method for producing an oral preparation containing water-soluble chitosan.
According to claim 1, in the step (S1-2), acetic anhydride is added to the liquid dissolved after performing the step (S1-1), stirred for 1 hour, and then 12 g of KOH is dissolved in 100 ml of water and added. Next, 2 ml of acetic anhydride was added again and stirred for 20 minutes, and then 6 g of KOH was dissolved in 50 ml of water and stirred for 1 hour. At this time, the amount of acetic anhydride was in the range of 20 to 40% of the weight of chitosan. Method of manufacturing the formulation.
According to claim 1, after performing the step (S1-2), 20 ml of a diluted solution of 1 g of KOH is added to the solution after stirring, and a primary neutralization reaction is carried out in a bath at 36° C. until the pH reaches 4. A method for producing an oral preparation containing water-soluble chitosan, characterized in that it undergoes a process.
According to claim 1, in the step (S1-4), after the primary neutralization reaction, 1 liter of distilled water in which 7 ml of acetic anhydride and 0.3 g of KOH are dissolved is added, and pH is reached in a bath at 36°C. A method for producing an oral preparation containing water-soluble chitosan, characterized in that it undergoes a secondary neutralization reaction for 2 hours until it becomes soluble.
The method of claim 6, wherein the mouthwash raw material includes a material selected from the group consisting of saponin, green tea extract, propolis, xylitol, and enzyme-treated stevia.
The method of claim 7, wherein the mouthwash raw material is mixed with the clean aqueous solution obtained through the step (S2-3), wherein the mouthwash raw material contains 4.0% by weight of saponin when the total weight of the mixture is 100% by weight. , A method for producing an oral preparation containing water-soluble chitosan, characterized in that 0.5% by weight of propolis and 2.8% by weight of xylitol are mixed with a stabilized aqueous solution.
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