JP2022085808A - Animal shampoo with antibacterial function and manufacturing method thereof - Google Patents
Animal shampoo with antibacterial function and manufacturing method thereof Download PDFInfo
- Publication number
- JP2022085808A JP2022085808A JP2021015100A JP2021015100A JP2022085808A JP 2022085808 A JP2022085808 A JP 2022085808A JP 2021015100 A JP2021015100 A JP 2021015100A JP 2021015100 A JP2021015100 A JP 2021015100A JP 2022085808 A JP2022085808 A JP 2022085808A
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- JP
- Japan
- Prior art keywords
- agent
- shampoo
- antibacterial
- thickener
- antibacterial function
- 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.)
- Granted
Links
- 239000002453 shampoo Substances 0.000 title claims abstract description 99
- 241001465754 Metazoa Species 0.000 title claims abstract description 43
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
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- 239000003429 antifungal agent Substances 0.000 claims abstract description 53
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- 229940073507 cocamidopropyl betaine Drugs 0.000 claims abstract description 45
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Classifications
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- A—HUMAN NECESSITIES
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- 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
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
- A61K8/442—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof substituted by amido group(s)
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- 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
- A61K8/46—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
- A61K8/466—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur containing sulfonic acid derivatives; Salts
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- 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
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/494—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with more than one nitrogen as the only hetero atom
- A61K8/4946—Imidazoles or their condensed derivatives, e.g. benzimidazoles
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- 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
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/494—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with more than one nitrogen as the only hetero atom
- A61K8/496—Triazoles or their condensed derivatives, e.g. benzotriazoles
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/005—Antimicrobial preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/10—Washing or bathing preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q5/00—Preparations for care of the hair
- A61Q5/02—Preparations for cleaning the hair
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/48—Thickener, Thickening system
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/70—Biological properties of the composition as a whole
- A61K2800/72—Hypo-allergenic
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Abstract
Description
本発明は、ペットの日用化粧品洗浄剤分野に関する。より具体的には、抗菌機能を有する動物シャンプー及びその製造方法に関する。 The present invention relates to the field of daily cosmetic cleaning agents for pets. More specifically, the present invention relates to an animal shampoo having an antibacterial function and a method for producing the same.
生活水準の向上に伴い、家庭で飼育するペットの数は絶えず増加し、近年、ペット皮膚病は臨床で最もよく見られる疾患の一つとなり、真菌及び細菌感染による皮膚病は相当な割合を占めた。過度に密集したペットの飼育、抗生剤の濫用、不合理な栄養摂取、人間用シャンプーのペットへの濫用などが、ペット皮膚疾患の発病率の上昇の誘因となっている。このような皮膚病の病因は複雑で、確診しにくく、治療に一定の難度があり、しかも再発率が比較的高い。 With increasing living standards, the number of pets kept at home is constantly increasing, and in recent years pet skin disease has become one of the most common clinical diseases, with fungal and bacterial infections accounting for a significant proportion. rice field. Overcrowding of pets, abuse of antibiotics, unreasonable nutrition, and abuse of human shampoo in pets have contributed to the increased incidence of pet skin diseases. The etiology of such skin diseases is complex, difficult to confirm, difficult to treat, and has a relatively high recurrence rate.
現在、一般的な皮膚疾患の治療は主に局部治療薬物の使用或いは全身治療薬物と組合せて使用する。そのうち局部治療薬物はより重要な地位を占有し、それは直接真菌を殺すか、皮膚の局部の微環境を変えることによって真菌の繁殖を抑制することができる。臨床的には、局所治療薬物は、発症初期には、多くの場合、効果は良好であり、同時に局所予防薬の使用は、疾患の再発予防に有用であると発見した。現在、ペット皮膚病を治療する常用薬物の形式はシャンプー、洗浄液、スプレー、軟膏、クリームとゲル剤などがあり、例えば、特許文献CN108451784Aは、チモール、抗菌剤、抗真菌剤を活性物質として製造された動物用抑菌シャンプーを公開した。しかし、このシャンプー体系では、抗真菌剤は難溶であることが多いが、水、ジメチルスルホキシド、エタノール、プロピレングリコール、ピロリドン、ジメチルホルムアミド及びイソプロパノールなどの溶剤を使用しても抗真菌剤を完全に溶解することができないため、抗菌剤の効果をうまく発揮することができず、また、「化粧品安全技術規範」の規定によると、ジメチルスルホキシド等の皮膚に有害な試薬はシャンプーに使用してはいけない。同時に、このシャンプーはグルコン酸クロルヘキシジン、酢酸クロルヘキシジンなどの抗菌剤を採用し、その稠度自体が劣っているが、エタノール、プロピレングリコールなどの多くが消泡剤としたアルコール類物質の添加は、シャンプー体系に、増稠が困難であり、気泡能力が低いなどの問題を発生させやすい。 Currently, the treatment of common skin disorders is mainly used with the use of local therapeutic agents or in combination with systemic therapeutic agents. Of these, local therapeutic drugs occupy a more important position, which can suppress fungal growth by directly killing the fungus or by altering the local microenvironment of the skin. Clinically, it has been found that topical drugs are often effective in the early stages of onset, while the use of topical prophylaxis is useful in preventing recurrence of the disease. Currently, the forms of commonly used drugs for treating pet skin diseases include shampoos, cleaning solutions, sprays, ointments, creams and gels. For example, Patent Document CN108451784A is manufactured using Timor, antibacterial agents and antifungal agents as active substances. Released an antibacterial shampoo for animals. However, in this shampoo system, antifungal agents are often sparingly soluble, but even with solvents such as water, dimethyl sulfoxide, ethanol, propylene glycol, pyrrolidone, dimethylformamide and isopropanol, the antifungal agents are completely dissolved. Since it cannot be dissolved, the effect of the antibacterial agent cannot be exerted well, and according to the provisions of the "Cosmetic Safety Technical Code", dimethyl sulfoxide and other harmful reagents to the skin should not be used in shampoo. .. At the same time, this shampoo uses antibacterial agents such as chlorhexidine gluconate and chlorhexidine acetate, and its consistency itself is inferior. In addition, it is difficult to increase the density, and problems such as low bubble capacity are likely to occur.
従来技術における欠点に対して、本発明は、抗菌薬物に対して良好な溶解能力を有し、抗菌剤の抗菌消炎作用を最大限に発揮することができる動物シャンプーを提供することを目的とし、作製した動物シャンプーは稠度が理想的であり、発泡作用が強く、温和で刺激がないという効果を有する。また、本発明は製造過程における安定性の問題を克服し、本発明の動物シャンプーは繰り返し凍結融解実験においても良好な安定性を有する。 In contrast to the shortcomings of the prior art, an object of the present invention is to provide an animal shampoo having a good dissolving ability for an antibacterial drug and capable of maximizing the antibacterial and anti-inflammatory action of the antibacterial agent. The prepared animal shampoo has an ideal consistency, has a strong foaming action, and has the effect of being mild and non-irritating. In addition, the present invention overcomes the problem of stability in the manufacturing process, and the animal shampoo of the present invention has good stability even in repeated freeze-thaw experiments.
本発明の目的は、抗菌機能を有する動物シャンプーを提供することである。 An object of the present invention is to provide an animal shampoo having an antibacterial function.
本発明の他の目的は上記動物シャンプーの製造方法を提供することである。 Another object of the present invention is to provide a method for producing the above animal shampoo.
本発明の上記目的は、以下の技術的な態様により実現される。 The above object of the present invention is realized by the following technical aspects.
抗菌機能を有する動物シャンプーであって、総質量部100部で、抗真菌剤1~5部、抗細菌剤1~5部、アルキルグリコシド4~16部、コカミドプロピルベタイン10~34部、複合増粘剤2~10部、キレート剤0.1~2部、調理剤1~5部、防腐剤0.01~1部、残量の脱イオン水の各成分を含む。 An animal shampoo with antibacterial function, with a total mass of 100 parts, 1 to 5 parts of antifungal agent, 1 to 5 parts of antibacterial agent, 4 to 16 parts of alkyl glycoside, 10 to 34 parts of cocamidopropyl betaine, composite. Contains 2 to 10 parts of thickener, 0.1 to 2 parts of chelating agent, 1 to 5 parts of cooking agent, 0.01 to 1 part of preservative, and each component of the remaining amount of deionized water.
好ましくは、前記アルキルグリコシドとコカミドプロピルベタインとの質量比は、6~16:10~30であり、両者の具体的な配合比率は6:30、8:26、10:22、12:18、14:14又は16:10であってもよい。 Preferably, the mass ratio of the alkyl glycoside to cocamidopropyl betaine is 6 to 16:10 to 30, and the specific compounding ratios of the two are 6:30, 8:26, 10:22, 12:18. , 14:14 or 16:10.
より好ましくは、前記アルキルグリコシドとコカミドプロピルベタインとの質量比は、6~10:22~30であり、両者の具体的な配合比率は6:30、8:26又は10:22である。 More preferably, the mass ratio of the alkyl glycoside to cocamidopropyl betaine is 6 to 10:22 to 30, and the specific compounding ratio of both is 6:30, 8:26 or 10:22.
動物の臨床によく見られる皮膚病を解決するために、本発明の成分には抗真菌と抗細菌の薬物成分が同時に含まれており、ペット表面の皮膚と毛髪を清潔にすると同時に、ペットによく見られる真菌性と細菌性皮膚病を治療することができる。しかし、当分野でよく使われる抗真菌剤はいずれも溶解しにくいので、本発明は大量の実験を通じて、アルキルグリコシド(APG)を主溶剤とし、コカミドプロピルベタイン(CAB)を助溶剤とする配合体系で抗真菌剤を溶解する方法が得られる。 In order to solve the skin diseases commonly seen in animal clinical practice, the ingredients of the present invention contain antifungal and antibacterial drug ingredients at the same time to clean the skin and hair on the pet surface and at the same time to make the pet pet. It can treat common fungal and bacterial skin diseases. However, since all of the antifungal agents often used in this field are difficult to dissolve, the present invention has been formulated with alkylglycoside (APG) as the main solvent and cocamidopropyl betaine (CAB) as the auxiliary solvent through a large amount of experiments. A systematic method of dissolving the antifungal agent is obtained.
APGは非イオン性表面活性剤であり、洗浄業界において乳化、発泡、洗浄の作用を発揮し、洗浄液、洗濯液、入浴液、洗剤、クレンザーエッセンス、金属洗浄剤の主要な活性成分である。CABは両性表面活性剤であり、良好な洗浄、泡立ち、調理の作用を有する。本研究の実験により、APG、CABをそれぞれ抗真菌剤の溶解とともに用量をだんだん増加し、その溶解速度は徐々に速くなるが、シャンプー全体の安定性は悪く、常温にしばらく置くと析出しやすいことを発見した。APGとCABを配合した後に、抗真菌剤の溶解速度は著しく向上したが、研究により、APG、CABはいかなる配合の比率でも良い安定性を有するものではなく、APG、CABの質量比は6~16:10~30の場合、シャンプーは繰り返し凍結融解の条件下でも良い安定性を示し、しかも良い発泡能力を持ち、泡は豊富で洗浄しやすい。 APG is a non-ionic surfactant that exerts emulsifying, foaming and cleaning actions in the cleaning industry and is the main active ingredient in cleaning solutions, washing solutions, bathing solutions, detergents, cleanser essences and metal cleaning agents. CAB is an amphoteric surfactant and has good cleaning, foaming and cooking effects. According to the experiment of this study, the doses of APG and CAB were gradually increased with the dissolution of the antifungal agent, and the dissolution rate gradually increased, but the stability of the shampoo as a whole was poor and it was easy to precipitate when left at room temperature for a while. I found. After blending APG and CAB, the dissolution rate of the antifungal agent improved significantly, but studies have shown that APG and CAB do not have good stability at any blending ratio, and the mass ratio of APG and CAB is 6 to. At 16:10 to 30, the shampoo shows good stability under repeated freeze-thaw conditions, yet has good foaming ability, and the foam is abundant and easy to wash.
好ましくは、前記配合増粘剤は、アミノ酸増粘剤とαオレフィンスルホン酸ナトリウムとが質量比2:0.1~5で配合形成される。 Preferably, the compounded thickener is formed by blending an amino acid thickener and sodium α-olefin sulfonate in a mass ratio of 2: 0.1 to 5.
最も好ましくは、前記配合増粘剤は、アミノ酸増粘剤とαオレフィンスルホン酸ナトリウムとが質量比1:1である。 Most preferably, the compounded thickener has an amino acid thickener and sodium α-olefin sulfonate in a mass ratio of 1: 1.
好ましくは、前記アミノ酸増粘剤は、セテアリルグルコシド、アクリレート共重合体エマルジョン(SF-1)、ヒドロキシプロピルメチルセルロース、ジオレイン酸メチルグルコース(DOE-120)、アルコールエーテルイソステアリン酸エステル及び脂肪ポリエチレングリコールエーテル(oxetal Vd-92)のうちの1種又は複数である。より好ましくは、ジオレイン酸メチルグルコース(DOE-120)、アルコールエーテルイソステアリン酸エステル及び脂肪ポリエチレングリコールエーテル(oxetal Vd-92)である。 Preferably, the amino acid thickener is cetearyl glucoside, acrylate copolymer emulsion (SF-1), hydroxypropylmethylcellulose, methylglucose dioleate (DOE-120), alcohol ether isostearic acid ester and fatty polyethylene glycol ether ( One or more of oxetal Vd-92). More preferably, it is methyl glucose dioleate (DOE-120), alcohol ether isostearate and fatty polyethylene glycol ether (oxetal Vd-92).
シャンプー体系は一般的に陰イオン系であるが、調合に添加した抗細菌剤、調理剤は陽イオン表面活性剤であるため、シャンプー体系の増粘が困難であるという問題を引き起こし、よく見られる高分子ポリマー系増粘剤は高温で変色しやすく、低温でゼリー化しやすく、表面活性剤の泡の豊富さを抑制し、清潔時の皮膚感は高分子原料に影響され、具体的に、べたつき感があり、洗浄してもきれいにならず、残留感が強い。また、光照射粘度が低下するなどの問題がある。そのため、以上の問題を解決するため、本発明は増粘剤を選択する時にアミノ酸増粘剤は増粘困難という問題を解決でき、しかも、溶液が澄んでおり、透明であるが、粘度を向上させることができない。従って、本発明は大量の実験を通して、革新的に、アミノ酸増粘剤と増粘に使用されていない表面活性剤αオレフィンスルホン酸ナトリウム(AOS)を、質量比2:0.1~5で配合した場合、増粘効果はアミノ酸増粘剤と他の増粘剤より優れた配合効果を有し、シャンプー体系を理想的な粘度に達させるだけでなく、製品もより安定しており、体系の泡の豊富さと洗浄感に影響を与えず、清浄時の肌感にも影響せず、べたつき感がなく、洗浄しやすく、重い残留感がない。 The shampoo system is generally anionic, but since the antibacterial agent and cooking agent added to the formulation are cationic surfactants, it causes a problem that it is difficult to thicken the shampoo system, which is often seen. High molecular polymer thickeners are prone to discoloration at high temperatures, easily jelly at low temperatures, suppress the abundance of foam in surfactants, and the skin feel at cleanliness is affected by the polymer raw materials, specifically, stickiness. There is a feeling, it does not clean even after washing, and there is a strong residual feeling. In addition, there is a problem that the viscosity of light irradiation is lowered. Therefore, in order to solve the above problems, the present invention can solve the problem that the amino acid thickener is difficult to thicken when selecting a thickener, and the solution is clear and transparent, but the viscosity is improved. I can't let you. Therefore, the present invention innovatively blends an amino acid thickener and a surface active agent α-olefin sulfonate sodium (AOS) not used for thickening in a mass ratio of 2: 0.1 to 5 through a large amount of experiments. If so, the thickening effect has a better compounding effect than amino acid thickeners and other thickeners, not only to bring the shampoo system to the ideal viscosity, but also to make the product more stable and systematic. It does not affect the abundance of foam and the feeling of washing, does not affect the feeling of the skin when cleaning, does not have a sticky feeling, is easy to wash, and does not have a heavy residual feeling.
好ましくは、前記抗真菌剤は、ケトコナゾール、硝酸エコナゾール、硝酸ミコナゾール、クロトリマゾール、フルコナゾールの1種又は複数種である。 Preferably, the antifungal agent is one or more of ketoconazole, econazole nitrate, miconazole nitrate, clotrimazole, and fluconazole.
好ましくは、前記抗細菌剤は、塩化ベンザルコニウム、臭化ベンザルコニウム、酢酸クロルヘキシジン、グルコン酸クロルヘキシジン、トリクロサン、ポリヘキサメチレンビグアニドのうちの1種又は複数種である。 Preferably, the antibacterial agent is one or more of benzalkonium chloride, benzalkonium bromide, chlorhexidine acetate, chlorhexidine gluconate, triclosan, and polyhexamethylene biguanide.
好ましくは、前記キレート剤は、エチレンジアミン、エチレンジアミン四酢酸(EDTA)、エチレンジァミン四酢酸ニナトリウム(EDTA-2Na)のうちの1種又は複数種である。 Preferably, the chelating agent is one or more of ethylenediamine, ethylenediaminetetraacetic acid (EDTA) and disodium ethylenediaminetetraacetate (EDTA-2Na).
好ましくは、前記調理剤は、セトリモニウムクロリド、ポリクオチニウム-7、カチオン性グアー、水溶性ラノリン、アミノシリコーン油、アミノシリコーン油マイクロエマルジョンのうちの1種又は複数種である。 Preferably, the cooking agent is one or more of cetrimonium chloride, polyquantinium-7, cationic guar, water-soluble lanolin, aminosilicone oil, and aminosilicone oil microemulsion.
好ましくは、前記防腐剤は安息香酸ナトリウム及び/又はイソチアゾリノンである。 Preferably, the preservative is sodium benzoate and / or isothiazolinone.
好ましい一態様では、本発明は、上記抗菌機能を有する動物シャンプーの製造方法を更に提供し、具体的には、
まずシャンプーの総体積の35%を占める脱イオン水を60~70℃まで加熱し、次にアルキルグリコシド、コカミドプロピルベタインを脱イオン水に加えて撹拌溶解し、完全に溶解した後に抗真菌剤を加え、60~70℃で加熱したまま、撹拌して溶解させ、抗真菌剤が十分溶解した後に調理剤を加え、調理剤が完全溶解した後に加熱を停止するステップ(1)と、
ステップ(1)に加熱を停止した後の冷却過程において、キレート剤を加えて撹拌して溶解し、40~50℃まで冷却すると抗細菌剤を加えて撹拌して溶解し、抗細菌剤が完全に溶解した後に、配合増粘剤を加えて撹拌して溶解し、配合増粘剤が完全に溶解した後に防腐剤と残量の脱イオン水を加えて均一に撹拌することで製品を得るステップ(2)とを含む。
In a preferred embodiment, the present invention further provides a method for producing an animal shampoo having the antibacterial function, specifically, the present invention.
First, deionized water, which occupies 35% of the total volume of shampoo, is heated to 60 to 70 ° C., then alkyl glycoside and cocamidopropyl betaine are added to the deionized water and dissolved by stirring. And the step (1) in which the mixture is stirred and dissolved while being heated at 60 to 70 ° C., the cooking agent is added after the antifungal agent is sufficiently dissolved, and the heating is stopped after the cooking agent is completely dissolved.
In the cooling process after stopping the heating in step (1), a chelating agent is added and stirred to dissolve, and when cooled to 40 to 50 ° C., an antibacterial agent is added and stirred and dissolved, and the antibacterial agent is completely dissolved. After dissolving in, add the compounded thickener and stir to dissolve, and after the compounded thickener is completely dissolved, add the preservative and the remaining amount of deionized water and stir evenly to obtain a product. (2) and is included.
好ましくは、ステップ(1)において、脱イオン水は65~70℃まで加熱する。
本発明の研究によると、製造プロセスは抗真菌剤の溶解効果に著しい影響を与え、例えば、ステップ(1)における抗真菌剤、アルキルグリコシド、コカミドプロピルベタイン、各原料の添加順は決して勝手にしてはならず、先にアルキルグリコシドとコカミドプロピルベタインを脱イオン水中に添加して溶解してから、順に抗真菌剤を添加した後、抗真菌剤の溶解速度は速くなり、かつ稠度が更に良くなる。また、加熱温度は抗真菌剤の溶解にも著しい影響を与え、加熱温度が30℃より低い場合、抗真菌剤はまったく溶解できないが、加熱温度が60~70℃の場合、溶解時間が短いだけでなく、シャンプーの粘度も良好である。
Preferably, in step (1), the deionized water is heated to 65-70 ° C.
According to the study of the present invention, the manufacturing process has a significant effect on the dissolving effect of the antifungal agent, for example, the order of addition of the antifungal agent, alkyl glycoside, cocamidopropyl betaine and each raw material in step (1) is never arbitrary. First, alkyl glycoside and cocamidopropyl betaine are added to the deionized water to dissolve them, and then the antifungal agents are added in order, and then the dissolution rate of the antifungal agents becomes faster and the consistency becomes higher. Get better. The heating temperature also has a significant effect on the dissolution of the antifungal agent. If the heating temperature is lower than 30 ° C, the antifungal agent cannot be dissolved at all, but if the heating temperature is 60 to 70 ° C, the dissolution time is short. Not only that, the viscosity of the shampoo is also good.
本発明は以下の有益な効果を有する。 The present invention has the following beneficial effects.
本発明は大量の実験を通じて、アルキルグリコシド(APG)を主溶剤とし、コカミドプロピルベタイン(CAB)を助溶剤として配合した後に、抗真菌成分の難溶問題をよく解決し、また、両者は特定の比率条件下で、シャンプー体系の安定性の問題を克服し、抗菌薬物に溶解効果を与え、シャンプー薬物にもっと良い抗菌効果を与えると同時に、シャンプーは繰り返し凍結融解条件下でも良好な安定性を有するようにする。また、革新的にアミノ酸増粘剤とAOSの配合で増粘剤を形成し、抗細菌剤による増粘困難という問題を克服し、シャンプー体系に理想的な稠度を達成させるとともに、従来の増粘剤がべたつき、安定性が悪いなどの多くの技術的問題を克服し、最終的に得られた動物のシャンプーは安定性が良く、発泡能力が強いなどの利点がある。 Through a large amount of experiments, the present invention well solved the problem of poor dissolution of antifungal components after blending alkyl glycoside (APG) as the main solvent and cocamidopropyl betaine (CAB) as the auxiliary solvent, and both were specified. Overcome the stability problem of the shampoo system under the ratio condition, give the antibacterial drug a dissolving effect, give the shampoo drug a better antibacterial effect, and at the same time, the shampoo has good stability even under repeated freeze-thaw conditions. To have. Innovatively, a thickener is formed by blending an amino acid thickener and AOS, overcoming the problem of difficulty in thickening due to an antibacterial agent, achieving ideal consistency for a shampoo system, and conventional thickening. Overcoming many technical problems such as stickiness and poor stability of the agent, the finally obtained animal shampoo has advantages such as good stability and strong foaming ability.
また、本発明の試験結果は、本発明のシャンプー体系の下で、適量の抗真菌剤、抗細菌剤を同時に添加することによって、抗菌に対する相乗効果を達成することができ、抗真菌剤の単独使用、抗細菌剤の単独使用より抗菌効果が顕著に優れていることを示す。 In addition, the test results of the present invention show that a synergistic effect on antibacterial activity can be achieved by simultaneously adding an appropriate amount of an antifungal agent and an antibacterial agent under the shampoo system of the present invention, and the antifungal agent alone. It shows that the antibacterial effect is remarkably superior to the use and the use of an antibacterial agent alone.
また、本発明の動物シャンプーの製造方法は簡単で、工業化しやすい。 Further, the method for producing an animal shampoo of the present invention is simple and easy to industrialize.
以下、具体的な実施に関連して本発明をさらに詳細に説明するが、実施例は本発明へのいかなる形の限定を構成しない。本発明に採用される試薬、方法および装置は、特に明記されていない限り、本技術分野における従来の試薬、方法および装置である。 Hereinafter, the present invention will be described in more detail in connection with specific embodiments, but the examples do not constitute any form of limitation to the present invention. Unless otherwise specified, the reagents, methods and devices used in the present invention are conventional reagents, methods and devices in the art.
特に明記されていない限り、以下の実施例に用いる試薬及び材料は市販のものである。 Unless otherwise specified, the reagents and materials used in the following examples are commercially available.
抗菌機能を有する動物シャンプー
本実施例は抗菌機能を有する動物シャンプーを提供し、総質量は100gで計算すると、
硝酸エコナゾール2g、グルコン酸クロルヘキシジン2g、アルキルグリコシド(APG)8g、コカミドプロピルベタイン(CAB)26g、エチレンジァミン四酢酸ニナトリウム(EDTA-2Na)0.1g、脂肪ポリエチレングリコールエーテル(oxetal Vd-92)2g、αオレフィンスルホン酸ナトリウム(AOS)2g、セントリモニウムクロリド1g、安息香酸ナトリウム0.1g、残量の脱イオン水の各成分で構成される。
上記の抗菌機能を有する動物シャンプーの製造方法は以下の通りである。
Animal shampoo with antibacterial function This example provides an animal shampoo with antibacterial function, and the total mass is calculated as 100 g.
Econazole Nitrate 2g, Chlorhexidine Gluconate 2g, Alkyl Glycoside (APG) 8g, Cocamidopropylbetaine (CAB) 26g, Ethylenediaminetetraacetic acid disodium (EDTA-2Na) 0.1g, Fat Polyethylene Glycol Ether (oxetal Vd-92) 2g , Α-olefin sodium sulfonate (AOS) 2 g, centrimonium chloride 1 g, sodium benzoate 0.1 g, and the remaining amount of deionized water.
The method for producing the above-mentioned animal shampoo having an antibacterial function is as follows.
(1)まず35mLの脱イオン水をビーカーに加え、70℃まで加熱し、続いてアルキルグルコシド8g、コカミドプロピルベタイン26gを脱イオン水中に加えて撹拌して溶解し、完全に溶解後に2gの硝酸エコナゾールを加え、70℃の加熱下で撹拌して溶解し、硝酸エコナゾールを十分に溶解した後、セトリモニウムクロリド1gを加えて加熱を停止し、 (1) First, 35 mL of deionized water was added to the beaker and heated to 70 ° C., then 8 g of alkyl glucoside and 26 g of cocamidopropyl betaine were added to the deionized water and dissolved by stirring. Add econazole nitrate, stir and dissolve under heating at 70 ° C. to fully dissolve econazole nitrate, then add 1 g of cetrimonium chloride to stop heating.
(2)ステップ(1)の冷却過程において、エチレンジァミン四酢酸ニナトリウム(EDTA-2Na)0.1gを加えて撹拌して溶解し、50℃まで冷却すると、グルコン酸クロルヘキシジン2gを加えて撹拌して溶解し、グルコン酸クロルヘキシジンが完全に溶解した後に配合増粘剤の脂肪ポリエチレングリコールエーテル(oxetal Vd-92)2gとαオレフィンスルホン酸ナトリウム(AOS)2gを加えて撹拌して溶解し、配合増粘剤が完全に溶解した後に安息香酸ナトリウム0.1gと残量の脱イオン水を加えて、均一に撹拌した後に分注して保存すればよい。 (2) In the cooling process of step (1), 0.1 g of disodium ethylenediaminetetraacetate (EDTA-2Na) was added and stirred to dissolve, and when cooled to 50 ° C., 2 g of chlorhexidine gluconate was added and stirred. After dissolution and complete dissolution of chlorhexidine gluconate, 2 g of fatty polyethylene glycol ether (oxetal Vd-92) and 2 g of α-olefin sulfonate sodium (AOS), which are compound thickeners, are added and stirred to dissolve, and the compound thickening is performed. After the agent is completely dissolved, 0.1 g of sodium benzoate and the remaining amount of deionized water may be added, and the mixture may be uniformly stirred and then dispensed and stored.
抗菌機能を有する動物シャンプー
本実施例は抗菌機能を有する動物シャンプーを提供し、総質量100gで計算すると、
硝酸ミコナゾール3g、酢酸クロルヘキシジン3g、アルキルグリコシド(APG)10g、コカミドプロピルベタイン(CAB)22g、エチレンジァミン四酢酸1g、アルコールエーテルイソステアリン酸エステル3gとαオレフィンスルホン酸ナトリウム(AOS)5g、カチオン性グアー3g、安息香酸ナトリウム0.1g、残量の脱イオン水の各成分で構成される。
上記の抗菌機能を有する動物シャンプーの製造方法は以下の通りである。
Animal shampoo with antibacterial function This example provides an animal shampoo with antibacterial function, and when calculated with a total mass of 100 g,
Myconazole nitrate 3 g, chlorhexidine acetate 3 g, alkyl glycoside (APG) 10 g, cocamidopropyl betaine (CAB) 22 g, ethylenediamine tetraacetic acid 1 g, alcohol ether isostearate 3 g and sodium α-olefin sulfonate (AOS) 5 g, cationic guar 3 g It is composed of 0.1 g of sodium benzoate and each component of the remaining amount of deionized water.
The method for producing the above-mentioned animal shampoo having an antibacterial function is as follows.
(1)まず35mLの脱イオン水をビーカーに入れて、65℃まで加熱し、次にアルキルグリコシド10g、コカミドプロピルベタイン22gを脱イオン水に加えて撹拌溶解し、完全に溶解した後に硝酸ミコナゾールを3g加え、65℃で加熱したまま、撹拌して溶解させ、硝酸ミコナゾールが十分溶解した後にカチオン性グアーを3g加えて、加熱を停止し、 (1) First, 35 mL of deionized water is placed in a beaker and heated to 65 ° C., then 10 g of alkyl glycoside and 22 g of cocamidopropyl betaine are added to the deionized water and dissolved by stirring. 3 g was added, and the mixture was stirred and dissolved while being heated at 65 ° C., and after the myconazole nitrate was sufficiently dissolved, 3 g of cationic guar was added to stop the heating.
(2)ステップ(1)の冷却過程において、エチレンジァミン四酢酸1gを加えて撹拌して溶解し、50℃まで冷却すると、酢酸クロルヘキシジン3gを加えて撹拌して溶解し、酢酸クロルヘキシジンが完全に溶解した後に配合増粘剤のアルコールエーテルイソステアリン酸エステル3gとαオレフィンスルホン酸ナトリウム(AOS)5gを加えて撹拌して溶解し、配合増粘剤が完全に溶解した後に安息香酸ナトリウム0.1gと残量の脱イオン水を加えて、均一に撹拌した後に分注して保存すればよい。 (2) In the cooling process of step (1), 1 g of ethylenediamine tetraacetic acid was added and stirred to dissolve, and when cooled to 50 ° C., 3 g of chlorhexidine acetate was added and stirred to dissolve, and chlorhexidine acetate was completely dissolved. Later, 3 g of alcohol ether isostearic acid ester and 5 g of α-olefin sulfonate sodium (AOS) were added and dissolved by stirring, and after the compounded thickener was completely dissolved, 0.1 g of sodium benzoate and the remaining amount were added. The deionized water of No. 1 may be added, and the mixture may be uniformly stirred and then dispensed and stored.
抗菌機能を有する動物シャンプー
本実施例は抗菌機能を有する動物シャンプーを提供し、総質量は100gで計算すると、
ケトコナゾール5g、塩化ベンザルコニウム5g、アルキルグリコシド(APG)6g、コカミドプロピルベタイン(CAB)30g、エチレンジァミン四酢酸ニナトリウム0.1g、ジオレイン酸メチルグルコース3gとαオレフィンスルホン酸ナトリウム(AOS)2g、アミノシリコーン油マイクロエマルジョン1g、イソチアゾリノン0.01g、残量の脱イオン水である。
上記の抗菌機能を有する動物シャンプーの製造方法は以下の通りである。
Animal shampoo with antibacterial function This example provides an animal shampoo with antibacterial function, and the total mass is calculated as 100 g.
5 g of ketoconazole, 5 g of benzalconium chloride, 6 g of alkyl glycoside (APG), 30 g of cocamidopropylbetaine (CAB), 0.1 g of disodium ethylenediamine tetraacetate, 3 g of methylglucose dioleate and 2 g of sodium α-olefin sulfonate (AOS), Aminosilicone oil microemulsion 1 g, isothiazolinone 0.01 g, and the remaining amount of deionized water.
The method for producing the above-mentioned animal shampoo having an antibacterial function is as follows.
(1)まず35mLの脱イオン水をビーカーに入れて、60℃まで加熱し、次にアルキルグリコシド12g、コカミドプロピルベタイン18gを脱イオン水に加えて撹拌溶解し、完全に溶解した後にケトコナゾールを5g加え、60℃で加熱したまま、撹拌して溶解させ、ケトコナゾールが十分溶解した後にアミノシリコーン油マイクロエマルジョンを1g加えて、加熱を停止し、 (1) First, 35 mL of deionized water is placed in a beaker and heated to 60 ° C., then 12 g of alkyl glycoside and 18 g of cocamidopropyl betaine are added to the deionized water and dissolved by stirring. Add 5 g and stir to dissolve while heating at 60 ° C. After the ketoconazole is sufficiently dissolved, add 1 g of aminosilicone oil microemulsion to stop heating.
(2)ステップ(1)の冷却過程において、エチレンジアミン四酢酸0.1gを加えて撹拌して溶解し、50℃まで冷却すると、塩化ベンザルコニウム5gを加えて撹拌して溶解し、塩化ベンザルコニウムが完全に溶解した後に配合増粘剤のジオレイン酸メチルグルコース3gとαオレフィンスルホン酸ナトリウム(AOS)2gを加えて撹拌して溶解し、配合増粘剤が完全に溶解した後にイソチアゾリノン0.01gと残量の脱イオン水を加えて、均一に撹拌した後に分注して保存すればよい。 (2) In the cooling process of step (1), 0.1 g of ethylenediamine tetraacetic acid was added and stirred to dissolve, and when cooled to 50 ° C., 5 g of benzalconium chloride was added and stirred to dissolve, and benzalco chloride was dissolved. After the nium is completely dissolved, 3 g of the compounded thickener, methyl glucose dioleate and 2 g of α-olefin sulfonate sodium (AOS) are added and stirred to dissolve, and after the compounded thickener is completely dissolved, 0.01 g of isothiazolinone is added. And the remaining amount of deionized water may be added, stirred uniformly, and then dispensed and stored.
溶剤の選別 Solvent sorting
1、コカミドプロピルベタイン(CAB)が抗真菌剤を溶解する用量の選別試験 1. Selection test of the dose of cocamidopropyl betaine (CAB) that dissolves the antifungal agent
(1)試験方法
シャンプー総体積を100mLとして計算し、まずビーカーに35mLの脱イオン水を加えて70℃まで加熱し、表1の中の各用量のコカミドプロピルベタイン(CAB)を秤量してビーカーに加えて撹拌溶解し、更に2gの抗真菌剤硝酸エコナゾールの原料を加え、最後に脱イオン水で満たし、温度は70℃の条件下で加熱撹拌する。各成分用量の選別試験の設計は表1に示す。
(2)評価指標:
溶解時間:抗真菌剤の添加から完全溶解までの時間、
泡の体積:撹拌法で、処方ごとに0.5gのサンプルを100mLメスシリンダーに入れて、20mLの純水を入れて、上下に100回ひっくり返して、1minの時に泡の体積の値を読み取る。
安定性実験:製造した処方によるサンプルを常温で置いて析出時間を統計する。
(2) Evaluation index:
Dissolution time: Time from addition of antifungal agent to complete dissolution,
Foam volume: Using the stirring method, put a 0.5 g sample for each formulation in a 100 mL graduated cylinder, add 20 mL of pure water, turn it upside down 100 times, and read the foam volume value at 1 min. ..
Stability experiment: Place the sample according to the prepared formulation at room temperature and statistics the precipitation time.
(3)試験結果
CAB用量の選別試験結果は表2を参照し、処方1は溶解せず、処方2~4は抗真菌剤を溶解する時間はいずれも長く、かつ常温放置条件で、抗真菌剤の析出時間は速すぎる。一方、処方5~6は溶解時間が短くて析出が遅く、いずれも析出する状況があるため、得られたシャンプーが不安定であることを表明し、CABに対する用量が大きいため、シャンプーの生産コストを増やす。
2、アルキルグルコシド(APG)溶解抗真菌剤の用量選別試験 2. Dose selection test for alkyl glucoside (APG) -dissolving antifungal agent
(1)試験方法
シャンプー総体積を100mLとして計算し、まずビーカーに35mLの脱イオン水を加えて70℃まで加熱し、表3の中の各比率アルキルグリコシド(APG)をビーカーに加えて溶解し、さらに2gの抗真菌剤硝酸エコナゾールの原料を加え、最後に脱イオン水を補い、温度は70℃の条件下で加熱撹拌する。各成分用量選別試験の設計を表3に示す。
(2)評価指標:
溶解時間:抗真菌剤の添加から完全溶解までの時間、
泡の体積:撹拌法で、処方ごとに0.5gのサンプルを100mLメスシリンダーに入れて、20mLの純水を入れて、上下に100回ひっくり返して、1minの時に泡の体積の値を読み取る。
安定性実験:製造した処方によるサンプルを常温で置いて析出時間を統計する。
(2) Evaluation index:
Dissolution time: Time from addition of antifungal agent to complete dissolution,
Foam volume: Using the stirring method, put a 0.5 g sample for each formulation in a 100 mL graduated cylinder, add 20 mL of pure water, turn it upside down 100 times, and read the foam volume value at 1 min. ..
Stability experiment: Place the sample according to the prepared formulation at room temperature and statistics the precipitation time.
(3)実験結果
APG用量の選別試験結果は表4を参照し、処方1-3は溶解せず、処方4は抗真菌剤を溶解する時間はいずれも長く、しかも抗真菌剤の析出時間は速すぎる。一方、処方5-7は溶解時間が短くて析出が遅く、いずれも析出する状況があるため、得られたシャンプーが不安定であることを表明し、APGに対する用量が大きいため、シャンプーの生産コストを増やす。
3、溶剤溶解抗真菌剤の選別試験 3. Sorting test for solvent-soluble antifungal agents
(1)試験方法:シャンプー総体積を100mLとして計算し、まずビーカーに35mLの脱イオン水を加えて70℃まで加熱し、表5の各異なる配合比率のヤシ油アミド(CAB)とアルキルグリコシド(APG)をビーカーに加えて溶解し、更に2gの抗真菌剤硝酸エコナゾール原料を加え、最後に脱イオン水を補充し、温度は70℃の条件下で加熱撹拌する。
(2)評価指標:
溶解時間:抗真菌剤の添加から完全溶解までの時間、
泡の体積:撹拌法で、処方ごとに0.5gのサンプルを100mLメスシリンダーに入れて、20mLの純水を入れて、上下に100回ひっくり返して、1minの時に泡の体積の値を読み取る。
安定性実験:製造した処方によるサンプルを常温で置いて析出時間を統計する。
(2) Evaluation index:
Dissolution time: Time from addition of antifungal agent to complete dissolution,
Foam volume: Using the stirring method, put a 0.5 g sample for each formulation in a 100 mL graduated cylinder, add 20 mL of pure water, turn it upside down 100 times, and read the foam volume value at 1 min. ..
Stability experiment: Place the sample according to the prepared formulation at room temperature and statistics the precipitation time.
(3)試験結果
各処方の溶解時間、泡体積、安定性試験の結果を記録し、表6に示す。
増粘剤の選別 Thickener selection
一、試験1 One, test 1
1、試験材料
抗真菌剤:硝酸エコナゾール;抗細菌剤:グルコン酸クロルヘキシジン;電解質類:塩化ナトリウム(NaCl)
高分子ポリマー類:カルボマー、カチオン性グアー;
アミノ酸増粘剤:脂肪ポリエチレングリコールエーテル(oxetal Vd-92)。
他の増粘剤:ヤシ油脂肪酸ジエタノールアミド(6501)、ポリグリコ-ル6000ジステアラート(638)、ヤシ油脂肪酸モノエタノールアミド(cmea)
1. Test material Antifungal agent: Econazole nitrate; Antibacterial agent: Chlorhexidine gluconate; Electrolytes: Sodium chloride (NaCl)
Polymers: Carbomer, Cationic Guar;
Amino acid thickener: Fat polyethylene glycol ether (oxetal Vd-92).
Other thickeners: coconut oil fatty acid diethanolamide (6501), polyglycol 6000 disteaert (638), coconut oil fatty acid monoethanolamide (cmea)
2、試験方法
シャンプー総体積を100mLとして計算し、まずビーカーに20mLの脱イオン水を加えて70℃まで加熱し、ビーカーに混ぜて溶解し、アルキルグリコシド(APG)8gとコカミドプロピルベタイン(CAB)26gを秤量してビーカーに混ぜて溶解し、更に2gの抗真菌剤の硝酸エコナゾール原料を加え、抗真菌剤の硝酸エコナゾールを完全に溶解した後に温度を下げて40℃ぐらいまで冷却してから抗細菌剤グルコン酸クロルヘキシジンを加えて撹拌して溶解し、グルコン酸クロルヘキシジンは完全に溶解した後に表7中の各増粘剤を加えて、完全に溶解するまで撹拌する。最後に脱イオン水で満たす。サンプルを製造した後、常温で放置して消泡させる。消泡後、粘度計でその粘度を測定し、シャンプーの放置消泡後の透明度を観察する。
2. Test method Calculate the total volume of shampoo as 100 mL, first add 20 mL of deionized water to the beaker, heat to 70 ° C, mix and dissolve in the beaker, and dissolve 8 g of alkyl glycoside (APG) and cocamidopropyl betaine (CAB). ) Weigh 26 g and mix in a beaker to dissolve, then add 2 g of the antifungal agent econazole nitrate, completely dissolve the antifungal agent econazole nitrate, then lower the temperature and cool to about 40 ° C. The antibacterial agent chlorhexidine gluconate is added and stirred to dissolve, and after the chlorhexidine gluconate is completely dissolved, each thickener in Table 7 is added and stirred until completely dissolved. Finally, fill with deionized water. After producing the sample, leave it at room temperature to defoam. After defoaming, measure the viscosity with a viscometer and observe the transparency of the shampoo after defoaming.
3、試験結果
各増粘剤試験結果の統計は表7に示す。
二、試験2
増粘剤Vd-92用量選別試験
Two, test 2
Thickener Vd-92 dose selection test
1、試験材料
アミノ酸増粘剤:脂肪ポリエチレングリコールエーテル(oxetal Vd-92)。
1. Test material Amino acid thickener: Fat polyethylene glycol ether (oxetal Vd-92).
2、試験方法
シャンプー総体積を100mLとして計算し、まずビーカーに35mLの脱イオン水を加えて70℃まで加熱し、ビーカーに混ぜて溶解し、アルキルグリコシド(APG)8gとコカミドプロピルベタイン(CAB)26gを秤量してビーカーに混ぜて溶解し、更に2gの抗真菌剤の硝酸エコナゾール原料を加え、抗真菌剤の硝酸エコナゾールを完全に溶解した後に温度を下げて40℃ぐらいまで冷却してから抗細菌剤グルコン酸クロルヘキシジンを加えて撹拌して溶解し、グルコン酸クロルヘキシジンは完全に溶解した後に異なる比率の増粘剤Vd-92を加えて、完全に溶解するまで撹拌する。最後に脱イオン水で満たす。サンプルを製造した後、常温で放置して消泡させる。消泡後、粘度計でその粘度を測定し、シャンプーの放置消泡後の透明度を観察する。
2. Test method Calculate the total volume of shampoo as 100 mL, first add 35 mL of deionized water to the beaker, heat to 70 ° C, mix and dissolve in the beaker, and dissolve 8 g of alkyl glycoside (APG) and cocamidopropyl betaine (CAB). ) Weigh 26 g and mix in a beaker to dissolve, then add 2 g of the antifungal agent econazole nitrate, completely dissolve the antifungal agent econazole nitrate, then lower the temperature and cool to about 40 ° C. The antibacterial agent chlorhexidine gluconate is added and stirred to dissolve, and after the chlorhexidine gluconate is completely dissolved, a different proportion of the thickener Vd-92 is added and stirred until completely dissolved. Finally, fill with deionized water. After producing the sample, leave it at room temperature to defoam. After defoaming, measure the viscosity with a viscometer and observe the transparency of the shampoo after defoaming.
3、試験結果増粘剤Vd-92用量選別の試験結果統計は表8に示す。
そこで本発明は、2gのアミノ酸増粘剤Vd-92を他の添加剤と共に増粘して併用したものであり、他の増粘剤の用量は表9、結果は表9に示す。
Therefore, in the present invention, 2 g of the amino acid thickener Vd-92 is thickened and used in combination with other additives, and the doses of the other thickeners are shown in Table 9 and the results are shown in Table 9.
製造プロセスの選別と最適化 Manufacturing process selection and optimization
1、抗真菌剤の溶解に最適な温度の選別試験 1. Selection test of the optimum temperature for dissolving antifungal agents
(1)シャンプーの総体積を100mLとして計算し、まず35mLの脱イオン水をビーカーに加え、表11のようにそれぞれ30℃、40℃、50℃、60℃、70℃、80℃、90℃まで加熱し、続いてアルキルグルコシド8g、コカミドプロピルベタイン26gを脱イオン水中に加えて撹拌して溶解し、完全に溶解後に2gの硝酸エコナゾールを加え、30℃、40℃、50℃、60℃、70℃、80℃、90℃で加熱したまま撹拌して溶解し、硝酸エコナゾールを十分に溶解した後、セトリモニウムクロリド1gを加えて加熱を停止し、 (1) Calculate the total volume of shampoo as 100 mL, first add 35 mL of deionized water to the beaker, and as shown in Table 11, 30 ° C, 40 ° C, 50 ° C, 60 ° C, 70 ° C, 80 ° C, 90 ° C, respectively. Then, 8 g of alkyl glucoside and 26 g of cocamidopropyl betaine were added to deionized water and dissolved by stirring. After complete dissolution, 2 g of econazole nitrate was added, and 30 ° C, 40 ° C, 50 ° C, 60 ° C. , 70 ° C., 80 ° C., 90 ° C. with stirring to dissolve, and after sufficiently dissolving econazole nitrate, add 1 g of cetrimonium chloride to stop heating.
(2)ステップ(1)の冷却過程において、エチレンジァミン四酢酸ニナトリウム(EDTA-2Na)0.1gを加えて撹拌して溶解し、50℃まで冷却すると、グルコン酸クロルヘキシジン2gを加えて撹拌して溶解し、グルコン酸クロルヘキシジンが完全に溶解した後に配合増粘剤の脂肪ポリエチレングリコールエーテル(oxetal Vd-92)2gとαオレフィンスルホン酸ナトリウム(AOS)2gを加えて撹拌して溶解し、配合増粘剤が完全に溶解した後に安息香酸ナトリウム0.1gと残量の脱イオン水を加えて、均一に撹拌した後に分注して保存すればよい。
抗真菌剤は添加から完全溶解までの時間及びシャンプーの全体粘度を観察し、統計結果は表11に示す。
The time from addition to complete dissolution of the antifungal agent and the overall viscosity of the shampoo were observed, and the statistical results are shown in Table 11.
2、異なる材料投入順によるシャンプーの製造実験
シャンプーの調合方法及びパラメータ条件は上記のプロセス5と同じである。
2. Shampoo manufacturing experiment with different material input order The shampoo preparation method and parameter conditions are the same as in Process 5 above.
(1)プロセス8
(1-1)シャンプーの総体積を100mLとして計算し、まず35mLの脱イオン水をビーカーに加え、70℃まで加熱し、続いて2gの硝酸エコナゾールを加え、70℃で加熱したまま、撹拌して、引き続きアルキルグルコシド8gとセトリモニウムクロリド1gを加え、10分間加熱撹拌してからコカミドプロピルベタイン26gを引き続き加えて、硝酸エコナゾールを完全に溶解した後、加熱を停止し、
(1-2)ステップ(1)の冷却過程において、エチレンジァミン四酢酸ニナトリウム(EDTA-2Na)0.1gを加えて撹拌して溶解し、50℃まで冷却すると、グルコン酸クロルヘキシジン2gを加えて撹拌して溶解し、グルコン酸クロルヘキシジンが完全に溶解した後に配合増粘剤の脂肪ポリエチレングリコールエーテル(oxetal Vd-92)2gとαオレフィンスルホン酸ナトリウム(AOS)2gを加えて撹拌して溶解し、配合増粘剤が完全に溶解した後に安息香酸ナトリウム0.1gと残量の脱イオン水を加えて、均一に撹拌した後に分注して保存すればよい。
(1) Process 8
(1-1) Calculate the total volume of shampoo as 100 mL, first add 35 mL of deionized water to the beaker, heat to 70 ° C, then add 2 g of econazole nitrate, and stir while heating at 70 ° C. Then, 8 g of alkyl glucoside and 1 g of cetrimonium chloride were continuously added, and after heating and stirring for 10 minutes, 26 g of cocamidopropyl betaine was continuously added to completely dissolve the econazole nitrate, and then the heating was stopped.
(1-2) In the cooling process of step (1), 0.1 g of disodium ethylenediamine tetraacetate (EDTA-2Na) was added and stirred to dissolve, and when cooled to 50 ° C., 2 g of chlorhexidine gluconate was added and stirred. After the chlorhexidine gluconate is completely dissolved, 2 g of the thickening agent fatty polyethylene glycol ether (oxetal Vd-92) and 2 g of sodium α-olefin sulfonate (AOS) are added, and the mixture is stirred and dissolved. After the thickener is completely dissolved, 0.1 g of sodium benzoate and the remaining amount of deionized water may be added, and the mixture may be uniformly stirred and then dispensed and stored.
(2)プロセス9
(2-1)シャンプーの総体積を100mLとして計算し、まず35mLの脱イオン水をビーカーに加え、70℃まで加熱し、続いてアルキルグリコシド8g、コカミドプロピルベタイン26gを脱イオン水に加えて撹拌して溶解し、完全に溶解した後に配合増粘剤の脂肪ポリエチレングリコールエーテル(oxetal Vd-92)2gとαオレフィンスルホン酸ナトリウム(AOS)2gを加え、配合増粘剤が完全に溶解した後に2gの硝酸エコナゾールを加え、70℃の加熱下で撹拌して溶解し、硝酸エコナゾールを十分に溶解した後、セトリモニウムクロリド1gを加えて加熱を停止し、
(2-2)ステップ(1)の冷却過程において、エチレンジァミン四酢酸ニナトリウム(EDTA-2Na)0.1gを加えて撹拌して溶解し、50℃まで冷却すると、グルコン酸クロルヘキシジン2gを加えて撹拌して溶解し、グルコン酸クロルヘキシジンが完全に溶解した後に安息香酸ナトリウム0.1gと残量の脱イオン水を加えて、均一に撹拌した後に分注して保存すればよい。
(2) Process 9
(2-1) Calculate the total volume of shampoo as 100 mL, first add 35 mL of deionized water to the beaker, heat to 70 ° C., and then add 8 g of alkyl glycoside and 26 g of cocamidopropyl betaine to the deionized water. After stirring and dissolving and completely dissolving, 2 g of the compounded thickener fatty polyethylene glycol ether (oxetal Vd-92) and 2 g of sodium α-olefin sulfonate (AOS) are added, and after the compounded thickener is completely dissolved. Add 2 g of econazole nitrate, stir and dissolve under heating at 70 ° C. to fully dissolve econazole nitrate, then add 1 g of cetrimonium chloride to stop heating.
(2-2) In the cooling process of step (1), 0.1 g of ethylenediaminetetraacetic acid disodium (EDTA-2Na) was added and stirred to dissolve, and when cooled to 50 ° C., 2 g of chlorhexidine gluconate was added and stirred. After the chlorhexidine gluconate is completely dissolved, 0.1 g of sodium benzoate and the remaining amount of deionized water may be added, and the mixture may be uniformly stirred and then dispensed and stored.
(3)シャンプー粘度と抗真菌剤の溶解時間
抗真菌剤は添加から完全溶解までの時間及びシャンプーの全体粘度を観察し、統計結果は表12に示す。
サンプル安定性試験 Sample stability test
一、影響因素試験
この実験は、加速実験よりも激しい条件下で行う。その目的は薬物の固有の安定性を検討し、その安定性に影響する要素及び可能な分解経路と分解産物を了解し、製剤の生産プロセス、包装、保管条件及び分解産物の分析方法に科学的な根拠を提供することである。「原料薬物と製剤安定性試験の指導原則」に従い、本製品の影響要素試験を行う。
1. Influential factor test This experiment is conducted under more severe conditions than the accelerated experiment. The purpose is to examine the inherent stability of the drug, understand the factors that affect its stability, possible degradation routes and degradation products, and scientifically analyze the production process, packaging, storage conditions and degradation products of the drug. To provide a good basis. Influential factor tests of this product will be conducted in accordance with the "Guidelines for Ingredient Drugs and Pharmaceutical Stability Testing".
1、試験器具と材料
30℃、40℃、60℃恒温箱、ライトチャンバー、密度瓶、粘度計、pH計、パイロットサンプル5本。
1. Test equipment and materials 30 ° C, 40 ° C, 60 ° C constant temperature box, light chamber, density bottle, viscometer, pH meter, 5 pilot samples.
2、試験方法
影響因素試験方案:実施例1、2、3のサンプルと増粘剤を添加しない比較サンプルを取り、市販要求で包装し、それぞれ常温、高温(60℃、40℃、30℃等)と強光(4500+500Lx)等の複数の条件で高温と強光影響因素試験を行い、10日放置し、それぞれ0日、5日、10日において有効抗真菌剤と抗細菌剤含量、シャンプーph、粘度、性状等の検出を行い、それを指標として試験サンプルの安定性を調べる。
3、試験結果
二、加速試験
この実験は加速条件の下で行う。その目的は薬物の化学あるいは物理変化を加速させ、薬物の安定性を検討し、製剤の設計、包装、運送、貯蔵に必要な資料を提供することである。
2. Accelerated test This experiment is conducted under accelerated conditions. Its purpose is to accelerate the chemical or physical changes of the drug, to study the stability of the drug, and to provide the necessary materials for the design, packaging, transportation and storage of the drug.
1、試験器具と材料
40℃恒温加速箱;密度瓶、粘度計、pH計、パイロットサンプル3ロット。
1. Test equipment and materials 40 ° C constant temperature acceleration box; density bottle, viscometer, pH meter, pilot sample 3 lots.
2、試験方法 2. Test method
3、実施例1の方法で製造され、抜取検査で合格したシャンプーの3ロットを取り、市販要求で包装され、40℃±2℃、相対湿度75%±5%の条件で6ヶ月間放置する。試験期間の0ヶ月目、1ヶ月目、2ヶ月目、3ヶ月目、6ヶ月目の月末にそれぞれサンプルを採取し、主成分含有量、ph、粘度、相対密度などの測定を行い、これを指標として試験サンプルの安定性を考察する。 3. Take 3 lots of shampoo manufactured by the method of Example 1 and pass the sampling inspection, packaged according to commercial requirements, and left for 6 months under the conditions of 40 ° C ± 2 ° C and relative humidity 75% ± 5%. .. Samples are taken at the end of the 0th, 1st, 2nd, 3rd, and 6th months of the test period, and the main component content, ph, viscosity, relative density, etc. are measured. Consider the stability of the test sample as an index.
3、実験結果
三、繰り返し凍結融解試験 3. Repeated freeze-thaw test
1、試験設備と材料
試験設備:-20℃冷蔵庫、40℃恒温加速培養箱、pH計、精密電子天秤、粘度計、高効率液体クロマトグラフ
材料:処方1、処方2サンプルと処方4(配合増粘剤を含まない)
1. Test equipment and materials Test equipment: -20 ° C refrigerator, 40 ° C constant temperature accelerated culture box, pH meter, precision electronic balance, viscometer, high-efficiency liquid chromatograph Material: Formula 1, Formula 2 Samples and Formula 4 (increased formulation) Does not contain adhesive)
2、試験方法:
製造した処方サンプルをまず-20℃で2d放置して、取り出して40℃の加速条件で2d放置する。3回循環し、サンプルを採取して処方の安定性状況を観察する。
2. Test method:
The prepared prescription sample is first left at −20 ° C. for 2d, then taken out and left at 40 ° C. for 2d. Circulate 3 times, take a sample and observe the stability of the formulation.
3、実験結果
動物シャンプーの体外抗真菌試験 In vitro antifungal test of animal shampoo
1、試験材料
マラセチア菌皮膚炎は近年、犬において重視され研究されている皮膚病であり、親油性の酵母様菌であり、正常な動物の皮膚表面に寄生できる。皮膚角質層と作用すると、癜風を引き起こし、皮膚毛包に侵入した後に毛嚢炎を引き起こし、近年、脂漏性皮膚炎の発病と関係があり、しかも痒みと紅斑は典型的な臨床症状であることが報告されている。そのため、本発明はマラセチア菌を試験菌株として動物シャンプーの抗真菌能力を測定する。
試験菌株は臨床で厚皮マラセチア菌を分離する。この3年間の実験室で、異なるペット病院、ホームレスペット基地の急性皮膚炎の犬の皮膚から分離した。
標準品質管理菌株は厚皮マラセチア菌である。
実施例1、実施例2、比較例1(成分と製造方法は実施例1と同じ、違いは抗細菌剤グルコース酸クロルヘキシジンを含まないことである)及び比較例2(成分は製造方法と実施例2と同じ、違いは抗細菌剤酢酸クロルヘキシジンを含まないことである)で製造した動物シャンプーを試験材料とし、対照として2組のブランクシャンプーを平行に設置する。
1. Test material Malassezia dermatitis is a skin disease that has been emphasized and studied in dogs in recent years, and is a lipophilic yeast-like bacterium that can parasitize the skin surface of normal animals. When acting on the stratum corneum of the skin, it causes tinea versicolor, folliculitis after invading the skin follicles, and has recently been associated with the development of seborrheic dermatitis, and itching and erythema are typical clinical symptoms. It has been reported. Therefore, the present invention measures the antifungal ability of animal shampoo using Malassezia bacterium as a test strain.
The test strain clinically isolates the thick-skinned Malassezia bacterium. In the laboratory for the last three years, they were isolated from the skin of dogs with acute dermatitis at different pet hospitals, homeless pet bases.
The standard quality control strain is Malassezia furfurin.
Example 1, Example 2, Comparative Example 1 (components and production method are the same as in Example 1, the difference is that the antibacterial agent chlorhexidine glucose acid is not contained) and Comparative Example 2 (components are production method and Example). Same as 2, the difference is that it does not contain the antibacterial agent chlorhexidine acetate), using animal shampoo as the test material, two sets of blank shampoos are installed in parallel as a control.
2、試験方法: 2. Test method:
(1)真菌分離
まず、70%のアルコールを使って、サンプリングする部位を消毒し、細菌汚染を防ぐ。その後、滅菌したピンセット又は止血クリップを用いて患部から毛髪を挟み、あるいはディスポーザブルブレードを用いて患側の皮屑を掻き取り、あるいは滅菌した毛ブラシを用いて患部の毛髪を整え、挟んだ毛屑、引っかけた皮屑、あるいは磨いた病患に罹る材料をLeeming&Notman培地に接種してマラセチア菌培養を行う。7~14日間培養し、50%PARKERインク染色鏡でマラセチア菌を確定した後、90mmの平板(同じ培地)で線を引いて単一コロニを分離し、単一コロニを取って同じ培養基の斜面で増菌保存する。
(1) Fungal isolation First, 70% alcohol is used to disinfect the sampled area to prevent bacterial contamination. Then, use sterilized tweezers or a hemostatic clip to pinch the hair from the affected area, or use a disposable blade to scrape the affected skin debris, or use a sterilized hair brush to trim the affected area and pinch the hair. Inoculate the Leeming & Notman medium with the caught skin debris or the polished material to be affected by the disease, and culture the Malassezia bacterium. After culturing for 7 to 14 days and confirming Malassezia furfurin with a 50% PARKER ink-staining mirror, draw a line on a 90 mm plate (same medium) to separate single colonies, take single colonies and slope the same culture group. Save the cells with enrichment.
(2)真菌同定および阻止円
菌種をSabouraud’s培地に接種し、32度の条件下で7-14日間培養し、成長できるのは厚皮マラセチア菌である。オックスフォードカップを培地に穴をあけ、動物シャンプーをオックスフォードカップに加え、相対側のオックスフォードカップにブランクシャンプーに加えて対照とし、32℃で24h培養して阻止円の大きさを観察する。
(2) Fungal identification and inhibition It is the thick-skinned Malassezia bacterium that can grow by inoculating the Sabouraud's medium with the fungal species and culturing under the condition of 32 degrees for 7-14 days. A hole is made in the medium of an Oxford cup, animal shampoo is added to the Oxford cup, and a blank shampoo is added to the opposite Oxford cup as a control, and the cells are cultured at 32 ° C. for 24 hours and the size of the inhibition circle is observed.
3、試験結果
各組の阻止円の大きさの統計結果を表20に示す。
動物シャンプーの体外抗細菌試験 In vitro antibacterial test of animal shampoo
1、試験材料
試験菌株:臨床で分離されたスタフィロコッカス・シュードインターメディウス。この3年間の実験室で、異なるペット病院、ホームレスペット基地の急性皮膚炎の犬の皮膚から分離した。
標準品質管理試験菌株:スタフィロコッカス・シュードインターメディウス。
実施例1、実施例2、比較例3(成分と製造方法は実施例1と同じ、違いは抗真菌剤硝酸エコナゾールを含まないことである)及び比較例4(成分は製造方法と実施例2と同じ、違いは抗真菌剤硝酸ミコナゾールを含まないことである)で製造した動物シャンプーを試験材料とし、対照として2組のブランクシャンプーを平行に設置する。
1. Test material Test strain: Clinically isolated Staphylococcus pseudointermedius. In the laboratory for the last three years, they were isolated from the skin of dogs with acute dermatitis at different pet hospitals, homeless pet bases.
Standard quality control test strain: Staphylococcus pseudointermedius.
Example 1, Example 2, Comparative Example 3 (Ingredients and production method are the same as in Example 1, the difference is that the antifungal agent econazole nitrate is not contained) and Comparative Example 4 (Ingredients are production method and Example 2). Same as above, the difference is that it does not contain the antifungal agent miconazole nitrate), using animal shampoo as the test material, and two sets of blank shampoos installed in parallel as a control.
2、試験方法
病理を採集、分離と精製した後、病原菌を保存する。試験開始後、品質管理菌株と同定した試験菌株を寒天平板に接種し、オックスフォードカップを用いて培地に穴をあけ、動物シャンプーをオックスフォードカップに加え、相対側のオックスフォードカップにブランクシャンプーを加えて対照とし、37℃で一晩培養を行った後、阻止円の大きさを観察する。
2. Test method After collecting, isolating and purifying the pathology, the pathogen is stored. After the start of the test, the test strain identified as the quality control strain was inoculated on an agar plate, a hole was made in the medium using an Oxford cup, animal shampoo was added to the Oxford cup, and blank shampoo was added to the opposite Oxford cup for control. After culturing at 37 ° C. overnight, observe the size of the blocking circle.
3、試験結果
各組の阻止円の大きさ結果の統計は表21に示す。
上記実施例は、本発明の好ましい実施形態であるが、本発明の実施形態は、上記実施例に限定されるものではなく、本発明の精神的実質と原理とを逸脱することなく他のいかなる変更、修飾、代替、組み合わせ、簡略化も、本発明の保護範囲に含まれるものでなければならない。
3. Test results Table 21 shows the statistics of the size of the blocking circles of each set.
The above-described embodiment is a preferred embodiment of the present invention, but the embodiment of the present invention is not limited to the above-mentioned embodiment, and any other embodiment of the present invention is not deviated from the spiritual substance and the principle. Modifications, modifications, substitutions, combinations and simplifications must also be within the scope of the invention.
Claims (10)
まずシャンプーの総体積の35%を占める脱イオン水を60~70℃まで加熱し、次にアルキルグリコシド、コカミドプロピルベタインを脱イオン水に加えて撹拌溶解し、完全に溶解した後に抗真菌剤を加え、60~70℃で加熱したまま、撹拌して溶解させ、抗真菌剤が十分溶解した後に調理剤を加え、調理剤が完全溶解した後に加熱を停止するステップ(1)と、
ステップ(1)に加熱を停止した後の冷却過程において、キレート剤を加えて撹拌して溶解し、40~50℃まで冷却すると抗細菌剤を加えて撹拌して溶解し、抗細菌剤が完全に溶解した後に、配合増粘剤を加えて撹拌して溶解し、配合増粘剤が完全に溶解した後に防腐剤と残量の脱イオン水を加えて均一に撹拌することで製品を得るステップ(2)とを含むことを特徴とする製造方法。 The method for producing an animal shampoo having an antibacterial function according to any one of claims 1 to 9.
First, deionized water, which occupies 35% of the total volume of shampoo, is heated to 60 to 70 ° C., then alkyl glycoside and cocamidopropyl betaine are added to the deionized water and dissolved by stirring. And the step (1) in which the mixture is stirred and dissolved while being heated at 60 to 70 ° C., the cooking agent is added after the antifungal agent is sufficiently dissolved, and the heating is stopped after the cooking agent is completely dissolved.
In the cooling process after stopping the heating in step (1), a chelating agent is added and stirred to dissolve, and when cooled to 40 to 50 ° C., an antibacterial agent is added and stirred and dissolved, and the antibacterial agent is completely dissolved. After dissolving in, add the compounded thickener and stir to dissolve, and after the compounded thickener is completely dissolved, add the preservative and the remaining amount of deionized water and stir evenly to obtain a product. (2) A manufacturing method comprising.
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