CN114522130A - Composition with anti-dandruff effect and preparation method thereof - Google Patents

Composition with anti-dandruff effect and preparation method thereof Download PDF

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CN114522130A
CN114522130A CN202210231476.0A CN202210231476A CN114522130A CN 114522130 A CN114522130 A CN 114522130A CN 202210231476 A CN202210231476 A CN 202210231476A CN 114522130 A CN114522130 A CN 114522130A
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extract
mixture
composition
parts
ammonium chloride
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CN114522130B (en
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祝桂芳
陈立琼
顾铭
王苏举
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Shanghai Huanqiu Industrial Development Co ltd
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Shanghai Huanqiu Industrial Development Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics 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
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9794Liliopsida [monocotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/40Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/41Amines
    • A61K8/416Quaternary ammonium compounds
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/4906Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with one nitrogen as the only hetero atom
    • A61K8/4926Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with one nitrogen as the only hetero atom having six membered rings
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics 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
    • A61K8/9755Gymnosperms [Coniferophyta]
    • A61K8/9761Cupressaceae [Cypress family], e.g. juniper or cypress
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
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    • A61K8/9789Magnoliopsida [dicotyledons]
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    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P17/00Drugs for dermatological disorders
    • A61P17/04Antipruritics
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P29/00Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier 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
    • A61Q17/005Antimicrobial preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/10Washing or bathing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/006Antidandruff preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/02Preparations for cleaning the hair
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/12Preparations containing hair conditioners
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
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Abstract

The invention provides a composition with an anti-dandruff effect and a preparation method thereof, and relates to the technical field of cosmetics. The composition comprises the piroctone olamine salt, the plant extract and the conditioner, and by controlling the components and the proportion of the piroctone olamine salt, the plant extract and the conditioner, the generation of dandruff can be better reduced by adopting a compounding mode, the cost performance is high, the allergy condition is not easy to occur, and the mildness is good; the composition can also nourish and care scalp and hair, and maintain scalp and hair health in multiple dimensions.

Description

Composition with anti-dandruff effect and preparation method thereof
Technical Field
The application relates to the technical field of cosmetics, in particular to a composition with an anti-dandruff effect and a preparation method thereof.
Background
Dandruff is a common disease of the scalp, known medically as "pityriasis capitis", which is clinically manifested by excessive fine, pale, dry or slightly greasy pieces of pityriasis capitis on the scalp or hair, which may be accompanied by itching, usually the process of desquamation of dead cells of the skin is manifested by separate clusters or flakes invisible to the naked eye, whereas in patients with dandruff it is manifested by a continuous, coherent aggregation, forming small fragments visible to the naked eye, and the only or typical symptom of certain skin diseases, such as seborrheic dermatitis, psoriasis and pityriasis rosea, is desquamation of the scalp. Dandruff can also occur in inflammatory skin diseases such as allergic dermatitis, discoid lupus erythematosus, lichen dermalis of the lichen type, and tinea capitis. Dandruff, pityriasis capitis and seborrheic dermatitis of the scalp are not strictly defined conceptually, and dandruff (pityriasis capitis) is generally considered to be mild non-inflammatory seborrheic dermatitis.
Researches show that the generation of dandruff is related to microbiological factors and local immune response, and long-term researches show that abnormal proliferation of malassezia is an important reason for causing the dandruff, so that the healthy microecology of the scalp can be maintained by adjusting the microecology balance of the scalp, the microbial infection of the scalp can be reduced, the excessive grease of the scalp can be further decomposed, and the seborrheic dermatitis can be improved.
Most of the anti-dandruff cosmetics sold in the market at present reduce the growth of scalp microorganisms, inhibit the transitional division of scalp keratinocytes, reduce the renewal speed of epidermis and prevent the cells to be exfoliated from accumulating into macroscopic massive scales by adding various antifungal medicaments as main functional components, thereby achieving the aim of removing dandruff. The anti-dandruff agent used in early stage comprises sulfur, salicylic acid, selenium disulfide, etc. Salicylic acid and tar are not designed for resisting fungi, so that the antifungal effect is not obvious, the dandruff removing effect is poor, the irritation is high, and the skin is easily damaged; the anti-dandruff cosmetic taking the selenium sulfide as the main functional component also has strong irritation, the hair feels rough after use, and if the hair is not washed thoroughly, the hair can lose hair and has peculiar smell. The addition of zinc pyrithione and climbazole, which are highly effective antifungal compounds, was later found to have a good effect on improving dandruff conditions, but zinc pyrithione has been banned from use in cosmetics in the european union due to the risk of carcinogenesis, whereas climbazole has a large environmental pollution in production and a low productivity.
And with the improvement of living standard of people, the safety of the components of the cosmetic composition becomes the focus of people's gradual attention, so people tend to mix antifungal medicines with the plant extract energy components to obtain a shampoo product with high safety and good effect, for example, as disclosed in Chinese patent application 202010297447.5, an anti-dandruff shampoo and a preparation method thereof are disclosed. The shampoo mainly comprises the following functional components: piroctone olamine salt, zinc-rich yeast extract, cacumen Platycladi extract, Ginseng radix extract, radix Sophorae Flavescentis extract, and D-panthenol. The shampoo uses the chemical anti-dandruff agent piroctone olamine salt and plant components with anti-dandruff and itching relieving effects, such as the cacumen biotae extract, the sophora flavescens root extract and the zinc-rich yeast extract, which are matched with each other to achieve more comprehensive anti-dandruff and itching relieving effects, and the ginseng root extract and the D-panthenol are added to provide nutrition for scalp and help hair to grow, but the shampoo is poor in mildness and low in cost performance.
For another example, chinese patent application 202011572346.0 discloses a shampoo with anti-dandruff and soothing effects, and a preparation method and applications thereof, wherein the shampoo comprises active raw materials such as 4-terpineol, melaleuca alternifolia leaf oil, willow flower/leaf/stem extract, illicium verum leaf extract, alteromonas ferment product, piroctone olamine salt, and auxiliary materials such as surfactant, cationic conditioner, ester-forming agent, thickener, humectant, and the like. The scalp micro-ecological environment can be fundamentally improved, the scalp is relieved, the irritation of the scalp is reduced, the water-oil balance of the scalp is adjusted, the metabolism of the scalp is promoted, and the effects of removing dandruff and relieving are remarkably achieved.
Therefore, there is a need to develop a composition which can better regulate the micro-ecological balance of scalp, has the effects of anti-inflammation, dandruff removal and itching relieving, and has good mildness, low irritation, high cost performance and wide application range.
Disclosure of Invention
Based on the defects in the prior art, the invention aims to provide a composition with an anti-dandruff effect and a preparation method thereof.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
the invention provides a composition with anti-dandruff efficacy, which comprises piroctone olamine salt, a plant extract, a conditioner and a solvent;
the mass ratio of the piroctone olamine salt to the plant extract to the conditioner is 1-2:0.8-1.5: 3.5-5;
preferably, the mass ratio of the piroctone olamine salt to the plant extract to the conditioner is 1.5-2:1-1.5: 3.8-5.
Still preferably, the mass ratio of the piroctone olamine salt, the plant extract and the conditioner is 2:1: 4.67.
The plant extract is selected from one or more of cacumen Platycladi extract, fructus Vitics Simplicifoliae extract, cortex Mori extract, Polygoni Multiflori radix extract, radix Sophorae Flavescentis extract, Ginseng radix extract and rhizoma Zingiberis recens extract;
preferably, the plant extract is selected from one or more of cacumen biotae extract, fructus viticis extract, cortex mori extract, sophora flavescens root extract and ginseng extract;
more preferably, the plant extract is selected from one or more of cacumen biotae extract, fructus viticis extract and cortex mori extract;
further preferably, the plant extract is a mixture of an extract of cacumen biotae, an extract of fructus viticis and an extract of cortex mori radicis;
still more preferably, the plant extracts are cacumen biotae extract, fructus viticis extract and cortex mori radicis extract in a mass ratio of 1-2:1: 1.
More preferably, the plant extract is an extract of cacumen biotae, an extract of fructus viticis and an extract of cortex mori radicis in a mass ratio of 2:1: 1.
The plant extract is prepared by the following method:
step 1, selecting dry cacumen biotae, fructus viticis or cortex mori radicis to remove impurities, and crushing to obtain cacumen biotae, fructus viticis or cortex mori radicis powder;
step 2, adding 95% ethanol into the cacumen biotae, fructus viticis or cortex mori powder obtained in the step 1 according to the mass ratio of 3:20(g/g), performing ultrasonic reflux extraction for 1-1.5 hours to obtain a crude extract, filtering the crude extract through a 100-mesh filter bag to obtain a filtrate, and concentrating the filtrate to 1/2 to obtain a concentrated solution 1;
step 3, passing the concentrated solution 1 obtained in the step 2 through a silica gel adsorption resin column, eluting with 75% ethanol, collecting and concentrating the eluent, and concentrating to 1/4-1/5 of the original volume to obtain a concentrated solution 2;
and 4, adding 1.2 times of propylene glycol into the concentrated solution obtained in the step 3, and uniformly stirring to obtain the extract of the cacumen biotae, the fructus viticis or the cortex mori radicis.
The composition also comprises a solvent, wherein the solvent is water or/and propylene glycol.
In some preferred embodiments, the composition comprises 10-20 parts by weight of piroctone olamine salt, 8-15 parts by weight of plant extract, 35-50 parts by weight of conditioner and 10-60 parts by weight of solvent.
Preferably, the composition comprises, by weight, 10-20 parts of piroctone olamine salt, 8-10 parts of plant extract, 38-47 parts of conditioner and 12-54 parts of solvent.
Still preferably, the composition comprises 20 parts by weight of piroctone olamine salt, 10 parts by weight of plant extract, 46.7 parts by weight of conditioner and 23.2 parts by weight of solvent.
The conditioner is selected from one or more of myristamidopropyl PG-dimethyl ammonium chloride phosphate and water mixture, linoleamidopropyl PG-dimethyl ammonium chloride phosphate, propylene glycol and water mixture, oleamidopropyl PG-dimethyl ammonium chloride, propylene glycol and water mixture, and behenamidopropyl dimethylamine and stearamidopropyl dimethylamine;
preferably, the conditioning agent is selected from one or more of myristamidopropyl PG-dimethyl ammonium chloride phosphate and water mixture, linoleamidopropyl PG-dimethyl ammonium chloride phosphate, propylene glycol and water mixture, and oleamidopropyl PG-dimethyl ammonium chloride, propylene glycol and water mixture.
Still preferably, the conditioner is prepared from the following components in parts by weight of 1-3:0-1:0-1 parts of a mixture of myristamidopropyl PG-dimethyl ammonium chloride phosphate and water, a mixture of linoleamidopropyl PG-dimethyl ammonium chloride phosphate, propylene glycol and water, and a mixture of oleamidopropyl PG-dimethyl ammonium chloride, propylene glycol and water.
Further preferably, the conditioner consists of a mixture of myristamidopropyl PG-dimethyl ammonium chloride phosphate and water, a mixture of linoleamidopropyl PG-dimethyl ammonium chloride phosphate, propylene glycol and water and a mixture of oleamidopropyl PG-dimethyl ammonium chloride, propylene glycol and water in a weight ratio of 2-3:1: 1.
Still further preferably, the conditioner consists of a mixture of myristamidopropyl PG-dimethyl ammonium chloride phosphate and water, a mixture of linoleamidopropyl PG-dimethyl ammonium chloride phosphate, propylene glycol and water and a mixture of oleamidopropyl PG-dimethyl ammonium chloride, propylene glycol and water in a weight part ratio of 2.67:1: 1.
The invention also provides a preparation method of the composition, which comprises the following steps:
(1) adding a solvent into a container, adding piroctone olamine salt and a conditioner under the stirring condition, heating and stirring until the mixture is completely dissolved, and controlling the temperature to be below 80 ℃ to obtain a mixture 1;
(2) and (3) the temperature of the mixture 1 is reduced to 40 ℃, the plant extract is added into the mixture 1 under the condition of stirring, and the mixture is uniformly stirred to obtain the composition.
The invention adopts a chemical anti-dandruff agent, a conditioner and a plant extract to prepare a composition with an anti-dandruff function, wherein the piroctone olamine salt is a high-efficiency anti-dandruff agent, the anti-dandruff mechanism is that an external channel generated by dandruff is fundamentally blocked through sterilization and antioxidation, so that dandruff and itching are effectively removed, but the dandruff is not temporarily removed from the appearance through degreasing and other modes, but the chemical anti-dandruff agent can cause dependence after long-term use, and the addition amount required by single use is higher, and the corresponding cost is higher. Therefore, the conditioner and the plant extract are added into the components, the scalp can be better maintained, the piroctone olamine salt, the conditioner and the plant extract can be better matched by controlling the specific components and the mass ratio in the composition, the addition amount of the piroctone olamine salt is reduced, the better anti-dandruff effect is achieved, the free radicals are reduced, and the scalp oxidation is resisted.
In addition, the application unexpectedly discovers that the composition prepared by mixing the piroctone olamine salt, the cacumen biotae extract, the fructus viticis extract, the cortex mori radicis extract and the conditioner has good antibacterial performance, mild performance and small irritation in the implementation process.
The invention also discloses the application of the composition in preparing washing and protecting products;
the washing and caring product comprises but is not limited to one or more of shampoo, hair conditioner and shower gel.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention provides a composition with an anti-dandruff effect, which comprises a chemical anti-dandruff agent, a conditioner and a plant extract, wherein the specific components and the mass ratio of the components are controlled, so that the components can be better matched, and the composition obtained by controlling the mass ratio of the piroctone olamine salt, the plant extract and the conditioner to be 1-2:0.8-1.5:3.5-5 and adopting a compounding mode can better reduce the generation of dandruff, has high cost performance, is not easy to cause allergy and is good in mildness.
The composition with the anti-dandruff effect is prepared by mixing multiple conditioners, so that the components have better interaction, and the stability of the product is ensured; the conditioner disclosed by the invention uses a mixture of myristamidopropyl PG-dimethyl ammonium chloride phosphate and water, a mixture of linoleamidopropyl PG-dimethyl ammonium chloride phosphate, propylene glycol and water and a mixture of oleamidopropyl PG-dimethyl ammonium chloride, propylene glycol and water in a weight ratio of 1-3:0-1:0-1 as a conditioner, and is mixed with a plant extract for use, so that the absorption of the plant extract in the composition by the scalp can be effectively improved, the micro-ecological environment of the scalp can be better adjusted, and the aims of hair care and hair nourishing are achieved.
(3) The composition provided by the invention can better reduce the generation of dandruff by adopting a compounding mode, and has the advantages of low irritation, high cost performance, difficulty in causing allergy and good mildness; the composition can also nourish and care scalp and hair, and maintain scalp and hair health in multiple dimensions.
Detailed Description
The present invention will be further illustrated in detail with reference to the following specific examples, which are not intended to limit the present invention but are merely illustrative thereof. The experimental methods used in the following examples are not specifically described, and the materials, reagents and the like used in the following examples are generally commercially available under the usual conditions without specific descriptions.
Figure BDA0003540711410000051
Figure BDA0003540711410000061
Method for preparing plant extract of basic example
Step 1, selecting dry cacumen biotae, fructus viticis or cortex mori radicis to remove impurities, and crushing to obtain cacumen biotae, fructus viticis or cortex mori radicis powder;
step 2, adding 95% ethanol into the cacumen biotae, fructus viticis or cortex mori powder obtained in the step 1 according to the mass ratio of 3:20(g/g), performing ultrasonic reflux extraction for 1-1.5 hours to obtain a crude extract, filtering the crude extract through a 100-mesh filter bag to obtain a filtrate, and concentrating the filtrate to 1/2 to obtain a concentrated solution 1;
step 3, passing the concentrated solution 1 obtained in the step 2 through a silica gel adsorption resin column, eluting with 75% ethanol, collecting and concentrating the eluent, and concentrating to 1/4-1/5 of the original volume to obtain a concentrated solution 2;
and 4, adding 1.2 times of propylene glycol into the concentrated solution obtained in the step 3, and uniformly stirring to obtain the extract of the cacumen biotae, the fructus viticis or the cortex mori radicis.
Example 1A composition having anti-dandruff effect
The paint comprises the following components in parts by weight:
20 parts of piroctone olamine salt, 10 parts of plant extract, 35.5 parts of SILKQUAT PTM, 34.5 parts of propylene glycol and 19.5 parts of water.
The plant extracts comprise cacumen biotae extract, fructus viticis extract and cortex mori extract in a mass ratio of 2:1: 1.
The preparation method comprises the following steps:
(1) adding a solvent into a container, adding piroctone olamine salt and a conditioner under the stirring condition, heating and stirring until the mixture is completely dissolved, and controlling the temperature to be below 80 ℃ to obtain a mixture 1;
(2) and (3) the temperature of the mixture 1 is reduced to 40 ℃, the plant extract is added into the mixture 1 under the condition of stirring, and the mixture is uniformly stirred to obtain the composition.
Example 2A composition having anti-dandruff effect
The paint comprises the following components in parts by weight:
15 parts of piroctone olamine salt, 14 parts of plant extract, 22.2 parts of SILKQUAT PTM, 13.3 parts of SILKQUAT EFA, 13.3 parts of SILKQUAT LC and 13.5 parts of propylene glycol.
Plant extracts: the weight ratio of the cacumen biotae extract to the fructus viticis extract to the cortex mori radicis extract is 1.5:1: 1.
The preparation method comprises the following steps: the same as in example 1.
Example 3A composition having anti-dandruff effect
The paint comprises the following components in parts by weight:
piroctone olamine salt 20 parts, plant extract 10 parts, SILKQUAT PTM 26.7 parts, SILKQUAT EFA 10 parts, SILKQUAT LC 10 parts, propylene glycol 23.3 parts;
the plant extracts comprise cacumen biotae extract, fructus viticis extract and cortex mori extract in a mass ratio of 2:1: 1.
The preparation method comprises the following steps: the same as in example 1.
Example 4A composition having anti-dandruff effect
The paint comprises the following components in parts by weight:
10 parts of piroctone olamine salt, 9 parts of plant extract, 22.2 parts of SILKQUAT PTM, 16.7 parts of SILKQUAT EFA and 23.1 parts of propylene glycol;
the plant extracts comprise cacumen biotae extract, fructus viticis extract and cortex mori extract in a mass ratio of 1:1: 1.
The preparation method comprises the following steps: the same as in example 1.
Comparative example 1
The difference from example 3 is that: the mass ratio of the piroctone olamine salt to the plant extract to the conditioner is 1:1:3, namely:
piroctone olamine salt 15.34 parts, plant extract 15.34 parts, SILKQUAT PTM 26.02 parts, SILKQUAT EFA 10 parts, SILKQUAT LC 10 parts, propylene glycol 23.3 parts;
the other operation steps are the same as in example 3.
Comparative example 2
The difference from example 3 is that: the mass ratio of the piroctone olamine salt to the plant extract to the conditioner is 3:1:6, namely:
piroctone olamine salt 23.01 parts, plant extract 7.67 parts, SILKQUAT PTM 26.02 parts, SILKQUAT EFA 10 parts, SILKQUAT LC 10 parts, propylene glycol 23.3 parts;
the other operation steps are the same as in example 3.
Comparative example 3
The difference from example 3 is that: SILKQUAT PTM, SILKQUAT EFA and SILKQUAT LC at a mass ratio of 1:2: 2; i.e., SILKQUAT PTM 9.34 parts, SILKQUAT EFA18.68 parts, and SILKQUAT LC 18.68 parts, and the other operational procedures were the same as in example 3.
Comparative example 4
The difference from example 3 is that:
the plant extract is a fructus viticis extract and a cortex mori radicis extract in a mass ratio of 2:1, and other operation steps are the same as the example 3.
Effect verification:
1. cosmetic eye irritation/Corrosion chick embryo chorioallantoic Membrane test
1.1 Experimental basis: inspection and quarantine industry Standard SN/T2309-2009 of the people's republic of China
1.2 purpose of experiment: the test substance is tested for its ability to induce changes in chick chorioallantoic membrane toxicity, and the criteria describe the elements and processes used to evaluate the potential ocular irritation of the substance being evaluated.
1.3 experimental principle: the chick embryo chorioallantoic membrane test is an early adopted method for the in vitro assessment of ocular irritation, where the chorioallantoic membrane (CAM) is a respiratory membrane that surrounds the chick embryo. The test utilizes the characteristics of complete, clear and transparent chorioallantoic membrane vascular system in the middle stage of the hatched chick embryo, a certain amount of test object is directly contacted with the chick embryo allantoic membrane, the change of chorioallantoic membrane toxicity effect indexes (such as bleeding, blood coagulation and blood vessel melting) is observed after a period of action, the indexes reflect the change of morphological structure, color and permeability of blood vessels and blood vessel network, and reflect the phenomena of chorioallantoic membrane protein denaturation and the damage degree thereof, and then a score is obtained by combination for evaluating the eye irritation of the test object.
1.4 Scoring criteria
Experiments performed using the reaction time method, using equation (1) to calculate the stimulation score (IS), the results retain two digits after the decimal point:
Figure BDA0003540711410000081
in the formula:
secH (bleeding time) -the average time to onset of bleeding observed on CAM membranes in seconds(s);
secL (vascular melting time) -the average time to onset of vascular melting observed on the CAM membrane in seconds(s);
secC (clotting time) -the average time to the onset of clotting observed on CAM membranes in seconds(s);
the ocular irritation of the test subjects was classified according to table 1 based on the calculated IS values.
TABLE 1 evaluation of stimulation scoring results
Figure BDA0003540711410000091
1.5 test purposes: simulating the irritancy of the anti-dandruff composition in shampoo.
1.6 preparation of simple shampoo:
the formula is as follows: DEHYTON PK45 ((mixture of cocamidopropyl betaine, sodium chloride and water): 1%, sample of the composition prepared according to the invention: 1%, water: to 100;
the reason for the simple shampoo formula setting is as follows: to minimize other interference factors, 1% DEHYTON PK45 was used in place of the shampoo base.
1.7 preparation of a solution to be detected: diluting the simple shampoo prepared in the step 1.6 by 100 times with deionized water to obtain liquid to be detected;
the reason for dilution is: the residence factor of shampoo in the product exposure information (exposure and residence factor) according to the guidelines for evaluating safety of cosmetics and their ingredients in the european union is 0.01, i.e., 1%.
1.8 test methods: reaction time method.
0.3mL of the solution to be tested is directly dripped on the surface of the CAM, the CAM reaction condition is observed, and the time of each toxic effect appearing within 5 minutes of the action is recorded.
The results of the irritation test of the compositions prepared in examples 1 to 4 of the present invention and comparative examples 1 to 4 are shown in Table 2 below.
TABLE 2 irritation Scoring results for compositions prepared in examples 1-4 and comparative examples 1-4
Serial number Experimental project The experimental results are as follows: and (4) evaluating the results:
1 example 1 0 Has no irritation
2 Example 2 0 Has no irritation
3 Example 3 0 Has no irritation
4 Example 4 0 Has no irritation
5 Comparative example 1 0 Has no irritation
6 Comparative example 2 1.21 Light irritation
7 Comparative example 3 1.05 Light irritation
8 Comparative example 4 0 Has no irritation
According to the detection results in the table 2, the anti-dandruff effect compositions prepared in the embodiments 1-4 of the invention are non-irritant, which shows that the compositions disclosed by the application are good in mildness and high in safety; while comparative examples 2-3 changing the mass ratio of piroctone olamine salt, plant extract and conditioner or increasing the content of conditioner increased the irritation of the composition, which resulted in a less irritating composition with reduced safety.
2. And (3) bacteriostatic test: MIC value test for Malassezia furfur
The test method comprises the following steps: the method is tested by referring to the minimum inhibitory concentration test (agar dilution method) of the Disinfection technical Specification-2.1.8.3 edition 2002 of Ministry of health.
During the experiment, samples are configured into different gradient concentrations (50ppm, 100ppm, 150ppm, 200ppm, 250ppm, 300ppm, 350ppm and 400ppm) to detect the bacteriostatic effect,
the test strains were: malassezia furfur (Malassezia furfur) with accession number ATCC 44344. The specific test results are shown in table 3 below.
Table 3 results of bacteriostatic tests on the compositions prepared in examples 1 to 4 and comparative examples 1 to 4
Figure BDA0003540711410000101
Figure BDA0003540711410000111
Note "+" indicates Malassezia furfur is present; "-" indicates that there is no malassezia furfur.
According to the detection results in the table 3 above, it can be seen that the compositions prepared in the examples and the comparative examples have certain bacteriostatic activity, and the bacteriostatic concentration detected in the example 1 is 250ppm, and the bacteriostatic concentration detected in the example 2 is 200 ppm; the bacteriostatic concentration of the sample in example 3 is 150ppm, and the bacteriostatic performance is the best; the inhibitory concentration of example 4 was 250 ppm; the bacteriostasis concentration of the conditioner in the comparative example 1 is 250ppm, the bacteriostasis is similar to that of the conditioner in the example 1, but the bacteriostasis is obviously inferior to that of the conditioner in the example 3, and the type of the conditioner and the proportion of the components have influence on the bacteriostasis concentration; the bacteriostatic concentration of comparative example 2 was 200ppm, but the composition was slightly irritating and less safe; the bacteriostatic concentration of comparative examples 3 and 4 was 300ppm, the bacteriostatic property was poor, and comparative example 3 had slight irritation; according to the detection results, the compositions prepared by the preferred technical scheme disclosed by the invention in the embodiments 2-3 are not irritant, have good antibacterial activity, and have good antibacterial performance at low concentration.
3. And (3) antioxidant test: evaluation of antioxidant Effect in vitro- -determination of DPPH free radical scavenging Capacity
3.1 test reagents and devices
Reagent: dpph (sigma), pbs (gibco), absolute ethanol (national reagent), vitamin c (cnw), absolute ethanol (national reagent).
Equipment: microplate reader (Tecan, Spark), micro oscillator (its Linbel, TS-92)
3.2 in vitro DPPH free radical scavenging test method
Preparing a sample into a solution to be detected with corresponding concentration, preparing a reaction system according to the addition amount of each reagent in the following table 4, and uniformly mixing, wherein 3 multiple holes and 1 background control hole are arranged at each concentration.
TABLE 4 DPPH radical scavenging test reaction System
Unit (μ L) C1 C2 T1 T2
DPPH ethanol solution 180 0 180 0
Liquid to be tested 0 0 20 20
Anhydrous ethanol 0 180 0 180
PBS 20 20 0 0
Note: the test solution is 1% of the anti-dandruff composition; the preparation method comprises the following steps: 1% of the antidandruff composition plus 99% of PBS buffer.
The reaction system was left at room temperature and was protected from light for 30 min. After the reaction was completed, the absorbance OD was read at 515nm, and the DPPH radical clearance of the sample was calculated according to the following formula (1).
Figure BDA0003540711410000112
In the formula:
c1-blank has absorbance value of DPPH system;
c2-blank absorbance value without DPPH system;
t1-sample set has absorbance value of DPPH system;
t2-absorbance values for sample set without DPPH system.
3.3 in vitro DPPH free radical scavenging test results, specific test results are shown in Table 5 below
TABLE 5
Item DPPH radical scavenging ratio (%)
Example 1 28.24
Example 2 36.13
Example 3 39.52
Example 4 28.42
Comparative example 1 30.54
Comparative example 2 29.67
Comparative example 3 28.58
Comparative example 4 27.72
As can be seen from the detection data in the above table 5, the compositions of the embodiments 2 to 3 of the present invention have a better DPPH radical scavenging rate, which indicates that the radical resistance of the composition can be significantly improved by reasonably controlling the content and the proportion of each component, thereby improving the oxidation resistance of the composition; while the types of the components are changed in the examples 1, 4 and the comparative examples 1-2, and the mixture ratio influences the antioxidant performance of the composition to a different degree, the antioxidant performance of the conditioner is changed in the comparative example 3, which is equivalent to the antioxidant performance of the examples 1 and 4, so that the antioxidant activity of the conditioner is not improved even if a plurality of conditioners are added, the mixture ratio of the conditioners is out of the protection range of the application, and the antioxidant performance of the composition is obviously influenced by the change of the types of the plant extracts in the comparative example 4.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A composition with anti-dandruff effect is characterized in that: the composition comprises piroctone olamine salt, a plant extract, a conditioner and a solvent, wherein the mass ratio of the piroctone olamine salt to the plant extract to the conditioner is 1-2:0.8-1.5: 3.5-5;
the conditioning agent is selected from one or more of myristamidopropyl PG-dimethyl ammonium chloride phosphate and water mixture, linoleamidopropyl PG-dimethyl ammonium chloride phosphate, propylene glycol and water mixture, oleamidopropyl PG-dimethyl ammonium chloride, propylene glycol and water mixture, and behenamidopropyl dimethylamine and stearamidopropyl dimethylamine.
2. The composition of claim 1, wherein: the mass ratio of the piroctone olamine salt to the plant extract to the conditioner is 1.5-2:1-1.5: 3.8-5.
3. The composition of claim 1, wherein: the plant extract is selected from one or more of cacumen Platycladi extract, fructus Vitics Simplicifoliae extract, cortex Mori extract, Polygoni Multiflori radix extract, radix Sophorae Flavescentis extract, Ginseng radix extract and rhizoma Zingiberis recens extract.
4. The composition of claim 3, wherein: the plant extracts are mixed according to the mass ratio of 1-2:1:1, an extract of cacumen biotae, an extract of fructus viticis and an extract of cortex mori radicis.
5. The composition of claim 1, wherein: the composition comprises, by weight, 10-20 parts of piroctone olamine salt, 8-15 parts of plant extract, 35-50 parts of conditioner and 10-60 parts of solvent.
6. The composition of claim 1, wherein: the conditioner consists of a mixture of myristamidopropyl PG-dimethyl ammonium chloride phosphate and water, a mixture of linoleamidopropyl PG-dimethyl ammonium chloride phosphate, propylene glycol and water and a mixture of oleamidopropyl PG-dimethyl ammonium chloride, propylene glycol and water in a weight ratio of 1-3:0-1: 0-1.
7. The composition of claim 6, wherein: the conditioner is composed of a mixture of myristamidopropyl PG-dimethyl ammonium chloride phosphate and water, a mixture of linoleamidopropyl PG-dimethyl ammonium chloride phosphate, propylene glycol and water and a mixture of oleamidopropyl PG-dimethyl ammonium chloride, propylene glycol and water in a mass ratio of 2.67:1: 1.
8. The composition according to any one of claims 1 to 7, characterized in that: the composition comprises the following components, by weight, 20 parts of piroctone olamine salt, 10 parts of plant extract, 26.7 parts of a mixture of myristamidopropyl PG-dimethyl ammonium chloride phosphate and water, 10 parts of a mixture of linoleamidopropyl PG-dimethyl ammonium chloride phosphate, propylene glycol and water, 10 parts of a mixture of oleamidopropyl PG-dimethyl ammonium chloride, propylene glycol and water and 23.3 parts of propylene glycol.
9. A method of preparing a composition according to any one of claims 1 to 8, characterized in that: the method comprises the following steps:
(1) adding a solvent into a container, adding piroctone olamine salt and a conditioner under the stirring condition, heating and stirring until the mixture is completely dissolved, and controlling the temperature to be below 80 ℃ to obtain a mixture 1;
(2) and (3) the temperature of the mixture 1 is reduced to 40 ℃, the plant extract is added into the mixture 1 under the condition of stirring, and the mixture is uniformly stirred to obtain the composition.
10. Use of a composition according to any one of claims 1 to 8 in the manufacture of a cleaning product.
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