CN115844786A - Plant anti-dandruff itching-relieving composition based on fermentation and preparation method and application thereof - Google Patents
Plant anti-dandruff itching-relieving composition based on fermentation and preparation method and application thereof Download PDFInfo
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- CN115844786A CN115844786A CN202211682598.8A CN202211682598A CN115844786A CN 115844786 A CN115844786 A CN 115844786A CN 202211682598 A CN202211682598 A CN 202211682598A CN 115844786 A CN115844786 A CN 115844786A
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Abstract
The invention discloses a preparation method of a plant anti-dandruff and anti-itching composition based on fermentation, which is characterized in that thyme, rosemary, swertia japonica and arnebia euchroma are pretreated to prepare powder; extracting the powder with the extracting solution, and filtering to obtain filtrate and filter residue; filtering the filtrate for the second time, and concentrating to obtain concentrated filtrate; fermenting the filter residue with lactobacillus, collecting supernatant, and concentrating to obtain filter residue fermentation liquid; mixing the concentrated filtrate with the residue fermentation broth to obtain herba Thymi vulgaris extract, herba Rosmarini officinalis extract, herba Swertiae Bimaculatae extract and Sinkiang radix Arnebiae extract, and mixing the extracts to obtain plant extract; mixing plant extractive solution, 2, 4-benzyl dichloroacrylate, sodium isostearoyl lactylate, sodium myristamidopropyl PG-dimethyl ammonium chloride phosphate, lactic acid, and 1, 3-propylene glycol uniformly to obtain the composition with dandruff removing and itching relieving effects. The plant anti-dandruff and anti-itching composition with high active ingredient content and good malassezia killing effect and anti-dandruff effect can be prepared by adopting the preparation method.
Description
Technical Field
The invention relates to the technical field of daily necessities, in particular to a preparation method of a plant anti-dandruff and anti-itching composition based on fermentation, the plant anti-dandruff and anti-itching composition prepared by adopting the preparation method and application of the plant anti-dandruff and anti-itching composition.
Background
Shampoo products have become a necessity in human daily life and are commonly used to clean and condition hair. With the increase of environmental pollution and living pressure of people, the endocrine system of the human body can be influenced, and the scalp and the hair can be adversely affected. More and more people are currently faced with problems such as hair loss, itching of the head, dandruff, etc. The existing dandruff removing agent for shampoo products mostly uses DMDMH hydantoin and carbazone as preservatives, and has large irritation to scalp, so that the problem of itching and dandruff of the head is caused. The dandruff is generated by two factors, one is that an external stimulus is contacted with the scalp to generate inflammation, skin cells are accelerated to proliferate, and dead skin is shed to cause dandruff, and the other is that the environment of the swan fungus colony is unbalanced, bacteria are bred in large quantity, and the scalp is itchy and intolerant. Therefore, inhibition of malassezia levels and the use of mild, low-irritation raw materials are critical to the treatment of dandruff. Pure chemical anti-dandruff ingredients such as Climbazole (CLM), piroctone Olamine (OCT), zinc Pyrithione (ZPT) and the like are generally used on the market.
Climbazole (CLM), commonly known as climbazole, is an antifungal compound that can combat fungi by inhibiting the synthesis of fungal cell membranes. The maximum use limit of climbazole in European Union is 2%, but the difference of the antidandruff and antipruritic effects of the climbazole is larger than that of ZPT and OCT, and the use amount is serious in downhill. ZPT is difficult to dissolve in water and uncomfortableFor clear products and at 11/3.2021, the european union committee formally issued a Regulation (EU) 2021/1902 code bulletin, revising the european cosmetic code annex II list of forbidden ingredients, wherein the anti-dandruff agent Zinc Pyrithione (ZPT) was added to it because of GHS classification of reproductive toxicity 1B; poor compatibility in Fe 3+ 、Cu 2+ The plasma can "discolor" and is incompatible with EDTA and nonionic surfactants. The aqueous OCT solution is colored to color the product and its cost is high.
In addition, the existing partial shampoo products use pure plant anti-dandruff agents, and because the composition of active ingredients of natural plants is very complex, when a certain active ingredient with an antibacterial effect is independently extracted, a very complex purification process is required, such as column chromatography and recrystallization; traditional plant extract is not separated and purified, and the content of active ingredients is very low, so that the effect of killing malassezia is not ideal, and the dandruff removing effect is poor.
Disclosure of Invention
The invention aims to provide a plant anti-dandruff and anti-itching composition based on fermentation and a preparation method thereof.
The invention also aims to provide the application of the plant anti-dandruff and anti-itching composition in shampoo products.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the present invention provides a method for preparing a fermentation-based plant anti-dandruff and anti-itch composition (refer to fig. 1), comprising the steps of:
s10, respectively pretreating and sieving fresh thyme, rosemary, swertia japonica and arnebia euchroma to prepare powder;
s20, adding the powder into the extracting solution respectively for extraction, and filtering to obtain filtrate and filter residue;
s30, concentrating the filtrate after secondary filtration to obtain concentrated filtrate; uniformly mixing the filter residue with water, adding lactobacillus for fermentation, collecting supernatant, and concentrating to obtain filter residue fermentation liquor;
s40, mixing the concentrated filtrate with the filter residue fermentation liquor to respectively prepare a thyme extracting solution, a rosemary extracting solution, a Japanese swertia herb extracting solution and a Sinkiang arnebia root extracting solution, and mixing the thyme extracting solution, the rosemary extracting solution, the Japanese swertia herb extracting solution and the Sinkiang arnebia root extracting solution to prepare plant extracting solutions;
s50, uniformly mixing the plant extract, 2, 4-benzyl dichloroacrylate, sodium isostearoyl lactylate, sodium myristamidopropyl PG-dimethyl ammonium chloride phosphate, lactic acid and 1, 3-propylene glycol to prepare the anti-dandruff and itching-relieving composition.
The plant sources of the plant anti-dandruff and itching-relieving composition are fresh thyme, rosemary, swertia japonica and arnebia euchroma which are pretreated to form powder respectively, plant active ingredients which are easy to dissolve out are extracted by using extract, and filter residues are fermented and extracted to obtain filter residue fermentation liquor. The secondary utilization of plant filter residue can obtain primary fermentation product or metabolite filtrate of lactobacillus fermentation, and the fermentation components contain abundant beneficial components such as amino acids and proteins, and can improve the effects of anti-inflammatory, itching relieving, soothing and antioxidant of shampoo products. The four plant components of the plant anti-dandruff itching-relieving composition are carried by the cationic surfactant in the composition, and are combined with hair after the cationic surfactant and hair anions attract each other in a yin-yang mode, so that the plant components are further combined with the hair and hair roots to further play an effective relieving and itching-relieving role, and the action mechanism is shown in figure 2. The prebiotics beneficial to human body is obtained by selecting plant filter residue for fermentation, and the bacterial colony balance of human scalp is controlled and regulated to achieve the effects of removing dandruff and relieving itching on the aspect of maintaining human scalp microecology.
The raw material of the plant anti-dandruff itching-relieving composition adopts 2, 4-benzyl dichloroacrylate as one of antibacterial components in the composition, and as shown in table 1, the composition has better water solubility and compatibility compared with the commercially available traditional 2, 4-dichlorobenzyl alcohol, thereby achieving more effective antibacterial and antiseptic effects.
TABLE 1 solubility and stability of modified 2, 4-dichlorobenzyl alcohols
The invention selects myristamidopropyl PG-dimethyl ammonium chloride sodium phosphate as a surfactant for keeping the stability of a finished preparation of the composition. Screening shows that the myristamidopropyl PG-dimethyl ammonium chloride sodium phosphate has better antibacterial synergistic effect than other surfactants. Comparative surfactants are: comparative 1-CAB-35 Cocoamidopropyl betaine, comparative 2-PEG-40 hydrogenated castor oil, comparative 3-sodium Cocoamidopropyl PG-dimethylammonium chloride phosphate, comparative 4-sodium fatty alcohol polyoxyethylene ether sulfate, comparative 5-fatty alcohol ammonium sulfate salt.
Since one of the unstable factors in the plant anti-dandruff and anti-itching composition is the precipitation of 2, 4-dichlorobenzyl alcohol, the test results refer to table 2 by using propylene glycol as a solvent, different surfactants as stabilizers, the conventional 2, 4-dichlorobenzyl alcohol as a solute and the water solubility thereof as evaluation indexes of the test.
TABLE 2 stability test of different surfactants on finished formulations
According to the invention, myristamidopropyl PG-dimethyl ammonium chloride sodium phosphate is selected as one of the raw materials, is not only used as a cationic surfactant, but also has a good synergistic effect on antibiosis, and refer to Table 3.
TABLE 3 minimum inhibitory concentration (in ppm) for different apparent activities
( Note: the minimum bacteriostatic concentration refers to the lowest bacteriostatic concentration of a test object when the test object has a bacteriostatic effect, and the lower the numerical value, the better the effect. )
The plant anti-dandruff and itching-relieving composition disclosed by the invention has the advantages that the sodium isostearoyl lactylate serving as a mild surfactant is selected as a raw material, the excellent moisturizing and skin moistening performances are realized, and meanwhile, the greasy feeling of the scalp caused by the silicon-oil-containing hair washing water can be improved by the composition in the application process.
Further, in step S50, the dandruff removing and itching relieving composition is prepared by using the following raw materials in parts by weight:
further, in step S50, the dandruff removing and itching relieving composition is prepared by using the following raw materials in parts by weight:
further, step S10 specifically includes: the method comprises the steps of drying fresh picked plants by hot air at 30-60 ℃, then crushing at-35-0 ℃, and sieving with a 300-mesh sieve to obtain plant powder.
As is known, the traditional Chinese medicine generates a large amount of heat in the crushing process to heat the material, so that high-temperature oxidation, deterioration and loss and segregation of effective components of heat-sensitive substances and bioactive substances in the material can occur, and the performance index of the heat-sensitive material is reduced or most of the heat-sensitive material is ineffective. In order to solve the problem of crushing, the invention adopts a JCWF-25C ultrafine crusher of Jinjun engineering machinery equipment limited company, utilizes an ultra-low temperature crushing technology, namely a cooling method while crushing, and a refrigerating machine with the temperature of-35 ℃ can be configured, so that softened or sticky medicines after temperature rise can be easily crushed, and bioactive components and various nutritional components which cannot resist high temperature can be kept, thereby improving the drug effect. By adopting an ultra-low temperature grinding technology, the average grain diameter of the materials is generally below 10um, the uniformity is improved, the color is consistent, and the powder is fine. By adopting ultra-low temperature pulverization technology, the purpose of ultrafine pulverization can be achieved for materials with high fiber, heat sensitivity, aromaticity, volatility and viscosity.
Further, step S20 specifically includes: respectively transferring the plant powder to an extraction tank, selecting a mixed solution of 1, 3-propylene glycol and water with a volume ratio of (1-5) to (1-5) as an extracting solution, extracting for 3 hours at 50-80 ℃ at 200-500 r/min, and filtering and separating to respectively obtain filtrate and filter residue.
Further, in step S30: in step S30: concentrating the filtrate to 1/2 of the original filtrate volume; mixing the filter residue with water according to a volume ratio of 1-1;
and (3) determining the total ammonia content of the obtained fermentation filtrate according to 'determination of total nitrogen in water quality alkaline potassium persulfate digestion ultraviolet spectrophotometry' (HJ 636-2012), taking the content of more than 0.3% as a concentration qualification judgment index, and if the content does not meet the content requirement, further concentrating the obtained fermentation filtrate until the content requirement is met.
Further, the Lactobacillus is selected from office of Ministry of health for hair-printing<List of strains available for food>The Lactobacillus specified in Notification (1) is obtained from the Collection of microorganisms of Guangdong province by fermenting a mixed strain. The lactobacillus is a mixed strain composed of Lactobacillus plantarum, lactobacillus rhamnosus, lactobacillus acidophilus and Bacillus bifidus, and has a concentration of 2 × 10 7 CUF/ml。
The lactobacillus plantarum is adopted as one of the strains to ferment the filter residue, so that the filter residue fermentation liquor has a certain immunoregulation effect and an inhibition effect on pathogenic bacteria, can reduce the serum cholesterol content and prevent cardiovascular diseases, and can maintain the flora balance in intestinal tracts, promote the absorption of nutrient substances, relieve lactose intolerance, inhibit the formation of tumor cells and the like. The lactobacillus rhamnosus is a probiotic which only generates L-lactic acid in the fermentation process and has no toxicity or side effect, has the functional characteristics of mainly regulating human flora, improving the discharge of human toxins and improving the immunity of organisms, and has higher application value. The filter residue fermentation liquor obtained by fermenting the lactobacillus acidophilus can activate macrophages, so that the defense capacity of an immune system to a host is improved; the bifidobacteria can not only generate acetic acid, but also synthesize various vitamins such as vitamin B2, folic acid and the like in fermentation, and can also activate the immune system of a human body, improve the anti-infection capacity of the human body, improve the oxidation resistance of cells, remove free radicals and other values.
Further, benzyl 2, 4-dichloroacrylate was prepared as follows:
adding 2, 4-dichlorobenzyl alcohol, dichloromethane and triethylamine into a three-neck flask provided with a condenser and a dropping funnel, starting mechanical stirring in an ice water bath, dropwise adding acryloyl chloride, continuing to react after the reaction is finished, filtering reaction liquid after the reaction is finished, extracting filtrate by using ethyl acetate, removing the ethyl acetate, and drying in a vacuum drying oven to obtain white powder solid, namely 2, 4-dichlorobenzyl acrylate;
wherein the molar ratio of the 2, 4-dichlorobenzyl alcohol to the acryloyl chloride to the triethylamine is 1.56.
In the present invention, the synthesis of benzyl 2, 4-dichloroacrylate is as follows:
the preparation method can improve the antibacterial property, solubility and stability of the 2, 4-dichlorobenzyl alcohol.
A plant composition for removing dandruff and relieving itching is prepared by the preparation method.
On the other hand, the invention provides the application of the plant anti-dandruff and anti-itching composition prepared by the preparation method in shampoo products. Such as shampoos, etc.
The invention has the beneficial effects that: the method comprises the steps of respectively pretreating fresh thyme, rosemary, swertia japonica and arnebia euchroma to form powder, extracting easily-dissolved plant active ingredients by using an extracting solution, and fermenting and extracting filter residues to obtain filter residue fermentation liquor. The fermented components obtained by secondary utilization of the plant filter residues contain rich amino acids, proteins and other beneficial components, and the anti-inflammatory, itching relieving, soothing and antioxidant effects of the shampoo product can be enhanced by selecting myristamidopropyl PG-dimethyl ammonium chloride sodium phosphate as a cationic surfactant and selecting benzyl 2, 4-dichloroacrylate for synergy.
Drawings
FIG. 1 is a process flow diagram of the preparation of the fermentation-based plant anti-dandruff anti-itch composition of the present invention.
FIG. 2 is a schematic diagram of the mechanism of removing dandruff and relieving itching of the plant composition for removing dandruff and relieving itching of the present invention.
FIG. 3 is a graph comparing the anti-dandruff and anti-itch effects of 0.1% OCT combined with 0.5% plant anti-dandruff and anti-itch composition and commercial shampoo Nos. 01-05 containing only 0.1% OCT.
Detailed Description
The technical solution of the present invention is further described below by way of specific embodiments.
Unless otherwise specified, various starting materials of the present invention are commercially available or prepared according to conventional methods in the art.
Example 1
The method comprises the steps of drying fresh picked plants (thyme, rosemary, swertia japonica and arnebia euchroma) by hot air at 40 ℃, respectively crushing by using a low-temperature crushing instrument (JCWF-25C ultrafine crusher) at-35 ℃, and sieving by using a 300-mesh sieve at the low temperature (-35 ℃) to obtain plant powder. Transferring the plant powder to the containerAnd an extraction tank, wherein 1, 3-propylene glycol and water (v: v = 1) are selected as extracting solutions, the extracting solutions are extracted for 3 hours at the rotation speed of 300r/min and the temperature of 70 ℃, and filter liquor and filter residues are obtained through filtration and separation respectively. Wherein the filtrate is ultrafiltered for the second time, and then the extract is concentrated to 1/2 volume; the filter residue was mixed with water (v: v = 1) and stirred uniformly with a stirring tank at 1000r/min, and cultured lactobacillus (2 x 10 7 CUF/ml), 210r/min, and fermenting at 31 ℃ for 12 hours. Centrifuging the obtained fermentation liquor by a high-speed centrifuge at 9000r/min for 25min, collecting supernatant, concentrating to 1/2 volume to obtain filter residue fermentation liquor, and measuring the total nitrogen content of the fermentation liquor: the nitrogen content of the thyme fermentation liquor is 0.332 percent; the nitrogen content of the rosemary herb fermentation liquor is 0.327 percent; the nitrogen content of the fermented liquid of the swertia japonica Makino is 0.376%; the nitrogen content of the Sinkiang arnebia root fermentation liquor is 0.346 percent. And finally mixing the obtained filtrate with the filter residue fermentation liquor to obtain thyme extract, rosemary extract, swertia japonica extract and arnebia euchroma extract.
Into a three-necked flask equipped with a condenser and a dropping funnel, 5.8g of dichlorobenzyl alcohol, 40mL of dichloromethane, and 3.5g of triethylamine were charged, and then a mechanical stirring was started in an ice water bath, and 4.64g of acryloyl chloride was added dropwise. After the dropwise addition is finished, reacting for 4 hours, filtering the reaction liquid, extracting with ethyl acetate, removing the solvent, and drying in a vacuum drying oven to obtain the benzyl 2, 4-dichloroacrylate.
Adding 4.2 parts of thyme extract, 12 parts of rosemary extract, 10 parts of swertia japonica extract, 10 parts of arnebia euchroma extract, 7 parts of benzyl 2, 4-dichloroacrylate, 10 parts of sodium isostearoyl lactylate, 10 parts of sodium myristamide propyl PG-dimethyl ammonium chloride phosphate, 1 part of lactic acid and 35.8 parts of 1, 3-propylene glycol into a stirring tank according to the mass fraction ratio, and stirring and mixing uniformly at 300r/min to obtain the plant anti-dandruff and anti-itching composition.
Example 2
The method comprises the steps of drying fresh picked plants (thyme, rosemary, swertia japonica and arnebia euchroma) by hot air at 40 ℃, respectively crushing by using a low-temperature crushing instrument (JCWF-25C ultrafine crusher) at-35 ℃, and sieving by using a 300-mesh sieve at the low temperature (-35 ℃) to obtain plant powder. Dividing the plant powder intoRespectively transferring to an extraction tank, selecting 1, 3-propylene glycol and water (v: v = 1) as extracting solution, extracting for 2h at the rotation speed of 200r/min and the temperature of 50 ℃, and filtering and separating to respectively obtain filtrate and filter residue. Wherein the filtrate is ultrafiltered for the second time, and then the extract is concentrated to 1/2 volume; the filter residue was mixed with water (v: v =1, 10), mixed well with a stirring tank at 500r/min, and cultured lactobacillus (2 x 10 7 CUF/ml), 210r/min, fermenting for 6h at 30 ℃. Centrifuging the obtained fermentation liquor for 25min at 8000r/min by using a high-speed centrifuge, collecting supernate, concentrating to 1/2 volume to obtain filter residue fermentation liquor, and measuring the total nitrogen content of the fermentation liquor: the nitrogen content of the thyme fermentation liquor is 0.322 percent; the nitrogen content of the rosemary herb fermentation liquor is 0.317 percent; the nitrogen content of the fermented liquid of the swertia japonica Makino is 0.366%; the nitrogen content of the Sinkiang arnebia root fermentation liquor is 0.336%. And finally, mixing the obtained filtrate with the filter residue fermentation liquor respectively to obtain thyme extract, rosemary extract, swertia japonica extract and arnebia euchroma extract.
To a three-necked flask equipped with a condenser and a dropping funnel, 5.8g of dichlorobenzyl alcohol, 40mL of dichloromethane, and 3.5g of triethylamine were added, and then a mechanical stirrer was started in an ice water bath, and 4.64g of acryloyl chloride was added dropwise. After the dropwise addition, the reaction is carried out for 4 hours again, the reaction solution is filtered, extracted by ethyl acetate, the solvent is removed, and the product is dried in a vacuum drying oven to obtain the 2, 4-dichloro benzyl acrylate.
Mixing 15 parts of thyme extract, 12 parts of rosemary extract, 10 parts of swertia japonica extract and 10 parts of arnebia euchroma extract, adding 7 parts of 2, 4-benzyl dichloroacrylate, 10 parts of sodium isostearoyl lactylate, 10 parts of sodium myristamide propyl PG-dimethyl ammonium chloride phosphate, 1 part of lactic acid and 35.8 parts of 1, 3-propylene glycol into a stirring tank according to the mass fraction ratio, and stirring and mixing uniformly at 300r/min to obtain the plant anti-dandruff and anti-itching composition.
Example 3
Drying fresh plants (thyme, herba Rosmarini officinalis, swertia japonica and radix Arnebiae of Sinkiang) with 40 deg.C hot air, pulverizing with-35 deg.C low temperature pulverizer (JCWF-25C ultra micro pulverizer) respectively, and sieving with 300 mesh sieve at low temperature (-35 deg.C) to obtain plant powder. Respectively transferring the plant powder to an extraction tank, selecting 1, 3-propylene glycol and water (v: v = 1) as extracting solution, extracting for 3h at the rotation speed of 400r/min and the temperature of 60 ℃, and filtering and separating to respectively obtain filtrate and filter residue. Wherein the filtrate is ultrafiltered for the second time, and then the extract is concentrated to 1/2 volume; the filter residue was mixed with water (v: v = 1) and stirred uniformly with a stirring tank at 1500r/min, and cultured lactobacillus (2 x 10 7 CUF/ml), 210r/min, fermenting for 12h at 35 ℃. Centrifuging the obtained fermentation liquid with a high speed centrifuge at 8000r/min for 25min, collecting supernatant, concentrating to 1/2 volume to obtain residue fermentation liquid, and measuring total nitrogen content of the fermentation liquid, wherein the nitrogen content of the thyme fermentation liquid is 0.302%; the nitrogen content of the rosemary herb fermentation liquid is 0.327 percent; the nitrogen content of the fermented liquid of the swertia japonica Makino is 0.355 percent; the nitrogen content of the Sinkiang arnebia root fermentation liquor is 0.341 percent. And finally, mixing the obtained filtrate with the filter residue fermentation liquor respectively to obtain thyme extract, rosemary extract, swertia japonica extract and arnebia euchroma extract.
To a three-necked flask equipped with a condenser and a dropping funnel, 5.8g of dichlorobenzyl alcohol, 40mL of dichloromethane, and 3.5g of triethylamine were added, and then a mechanical stirrer was started in an ice water bath, and 4.64g of acryloyl chloride was added dropwise. After the dropwise addition, the reaction is carried out for 4 hours again, the reaction solution is filtered, extracted by ethyl acetate, the solvent is removed, and the product is dried in a vacuum drying oven to obtain the 2, 4-dichloro benzyl acrylate.
Mixing 5 parts of thyme extract, 10 parts of rosemary extract, 10 parts of swertia japonica extract and 10 parts of arnebia euchroma extract, adding 7 parts of benzyl 2, 4-dichloroacrylate, 10 parts of sodium isostearoyl lactylate, 10 parts of sodium myristamide propyl PG-dimethyl ammonium chloride phosphate, 1 part of lactic acid and 37 parts of 1, 3-propylene glycol into a stirring tank according to the mass fraction ratio, and stirring and mixing uniformly at 300r/min to obtain the plant anti-dandruff and itching-relieving composition.
Example 4
Drying fresh plants (thyme, herba Rosmarini officinalis, swertia japonica and radix Arnebiae of Sinkiang) with hot air at 40 deg.C, pulverizing with-35 deg.C low temperature pulverizer (JCWF-25C ultra-fine pulverizer, jinan Jun engineering machinery Co., ltd.), and sieving with 300 mesh sieve at (-35 deg.C)Obtaining the plant powder. Respectively transferring the plant powder to an extraction tank, selecting 1, 3-propylene glycol and water (v: v = 1) as extracting solution, extracting for 3h at the rotation speed of 500r/min and the temperature of 80 ℃, and filtering and separating to respectively obtain filtrate and filter residue. Wherein the filtrate is ultrafiltered for the second time, and then the extract is concentrated to 1/2 volume; the filter residue was mixed with water (v: v = 1) and stirred uniformly with a stirring tank at 1000r/min, and cultured lactobacillus (2 x 10 7 CUF/ml), 210r/min, fermenting for 12h at 31 ℃. Centrifuging the obtained fermentation liquor by a high-speed centrifuge at 9000r/min for 25min, collecting supernatant, concentrating to 1/2 volume to obtain filter residue fermentation liquor, and measuring the total nitrogen content of the fermentation liquor: the nitrogen content of the thyme fermentation liquor is 0.344 percent; the nitrogen content of the rosemary herb fermentation liquor is 0.319 percent; the nitrogen content of the fermented liquid of the swertia japonica Makino is 0.380 percent; the nitrogen content of the Sinkiang arnebia root fermentation liquor is 0.336%. And finally, mixing the obtained filtrate with the filter residue fermentation liquor respectively to obtain thyme extract, rosemary extract, swertia japonica extract and arnebia euchroma extract.
Into a three-necked flask equipped with a condenser and a dropping funnel, 5.8g of dichlorobenzyl alcohol, 40mL of dichloromethane, and 3.5g of triethylamine were charged, and then a mechanical stirring was started in an ice water bath, and 4.64g of acryloyl chloride was added dropwise. After the dropwise addition, the reaction is carried out for 4 hours again, the reaction solution is filtered, extracted by ethyl acetate, the solvent is removed, and the product is dried in a vacuum drying oven to obtain the 2, 4-dichloro benzyl acrylate.
Mixing 3 parts of thyme extract, 12 parts of rosemary extract, 15 parts of swertia japonica extract and 15 parts of arnebia euchroma extract, adding 5 parts of 2, 4-benzyl dichloroacrylate, 10 parts of sodium isostearoyl lactylate, 15 parts of sodium myristamide propyl PG-dimethyl ammonium chloride phosphate, 1 part of lactic acid and 35.8 parts of 1, 3-propylene glycol into a stirring tank according to the mass fraction ratio, and stirring and mixing uniformly at 300r/min to obtain the plant anti-dandruff and anti-itching composition.
Example 5
Drying fresh plants (thyme, herba Rosmarini officinalis, swertia japonica and radix Arnebiae of Sinkiang) with 40 deg.C hot air, pulverizing with-35 deg.C low-temperature pulverizer (JCWF-25C ultra-fine pulverizer, jun horse engineering machinery Co., ltd.), and pulverizing at low temperatureSieving with 300 mesh sieve at (-35 deg.C) to obtain plant powder. Respectively transferring the plant powder to an extraction tank, selecting 1, 3-propylene glycol and water (v: v = 1) as extracting solutions, extracting for 3h at the rotation speed of 300r/min and the temperature of 70 ℃, and filtering and separating to respectively obtain filtrate and filter residue. Wherein the filtrate is ultrafiltered for the second time, and then the extract is concentrated to 1/2 volume; the filter residue was mixed with water (v: v = 1) and stirred uniformly in a stirred tank at 2000r/min, and cultured lactobacillus (2 x 10 7 CUF/ml), 210r/min, fermenting for 18h at 40 ℃. Centrifuging the obtained fermentation liquor by a high-speed centrifuge at 10000r/min for 25min, collecting supernatant, concentrating to 1/2 volume to obtain filter residue fermentation liquor, and measuring the total nitrogen content of the fermentation liquor: the nitrogen content of the thyme fermentation liquor is 0.324 percent; the nitrogen content of the rosemary herb fermentation liquor is 0.337 percent; the nitrogen content of the fermented liquid of the swertia japonica Makino is 0.326 percent; the nitrogen content of the Sinkiang arnebia root fermentation liquor is 0.386 percent. And finally, mixing the obtained filtrate with the filter residue fermentation liquor respectively to obtain thyme extract, rosemary extract, swertia japonica extract and arnebia euchroma extract.
Mixing 7 parts of thyme extract, 15 parts of rosemary extract, 15 parts of swertia japonica extract and 15 parts of arnebia euchroma extract, adding 7 parts of 2, 4-benzyl dichloroacrylate, 10 parts of sodium isostearoyl lactylate, 10 parts of sodium myristamide propyl PG-dimethyl ammonium chloride phosphate, 1 part of lactic acid and 20 parts of 1, 3-propylene glycol into a stirring tank according to the mass fraction ratio, and stirring and mixing uniformly at 300r/min to obtain the plant anti-dandruff and anti-itching composition.
Comparative example 1
Adding 7.5 parts of thyme extract, 15.3 parts of rosemary extract, 13.3 parts of Sinkiang arnebia root extract, 7.0 parts of modified-dichlorobenzyl alcohol, 10 parts of sodium isostearoyl lactylate, 10 parts of sodium myristamide propyl PG-dimethyl ammonium chloride phosphate, 1.0 part of lactic acid and 35.9 parts of 1, 3-propylene glycol into a stirring tank according to the mass fraction ratio, and uniformly stirring and mixing at 300r/min to obtain the plant anti-dandruff and anti-itching composition.
Wherein the preparation methods of the thyme extract, the rosemary extract and the arnebia euchroma extract are the same as those of the example 1.
Comparative example 2
Adding 7.5 parts of thyme extract, 15.3 parts of rosemary extract, 13.3 parts of swertia japonica extract, 7.0 parts of modified-dichlorobenzyl alcohol, 10 parts of sodium isostearoyl lactylate, 10 parts of sodium myristamide propyl PG-dimethyl ammonium chloride phosphate, 1.0 part of lactic acid and 35.9 parts of 1, 3-propylene glycol into a stirring tank according to the mass fraction ratio, and uniformly stirring and mixing at 300r/min to obtain the plant anti-dandruff and anti-itching composition.
The preparation method of the thyme extract, the rosemary extract and the swertia japonica extract is the same as that of example 1.
Comparative example 3
Adding 15.3 parts of rosemary herb extract, 13.3 parts of swertia japonica extract, 13.3 parts of arnebia euchroma extract, 7.0 parts of modified-dichlorobenzyl alcohol, 10 parts of sodium isostearoyl lactylate, 10 parts of sodium myristamide propyl PG-dimethyl ammonium chloride phosphate, 1.0 part of lactic acid and 35.9 parts of 1, 3-propylene glycol into a stirring tank according to the mass fraction ratio, and stirring and mixing uniformly at 300r/min to obtain the plant anti-dandruff and anti-itching composition.
Wherein the preparation methods of the rosemary herb extract, the swertia japonica extract and the arnebia euchroma extract are the same as those in example 1.
Comparative example 4
Adding 7.5 parts of thyme extract, 13.3 parts of swertia japonica extract, 13.3 parts of arnebia euchroma extract, 7.0 parts of modified-dichlorobenzyl alcohol, 10 parts of sodium isostearoyl lactylate, 10 parts of sodium myristamide propyl PG-dimethyl ammonium chloride phosphate, 1.0 part of lactic acid and 35.9 parts of 1, 3-propylene glycol into a stirring tank according to the mass fraction ratio, and stirring and mixing uniformly at 300r/min to obtain the plant anti-dandruff and anti-itching composition.
Wherein the preparation method of the thyme extract, the swertia japonica extract and the arnebia euchroma extract is the same as that of the example 1.
Comparative example 5
Drying fresh picked plants by hot air at 40 ℃, then crushing by using a special low-temperature crushing instrument at-35 ℃, and sieving by using a 300-mesh sieve at a low temperature to obtain plant powder. Transferring the plant powder to an extraction tank, selecting 1, 3-propylene glycol and water (v: v = 1) as an extracting solution, extracting for 3 hours at the rotation speed of 300r/min and the temperature of 70 ℃, and filtering and separating to obtain filtrate and filter residue respectively. Wherein the filtrate is ultrafiltered twice, and then the extract is concentrated to 1/2 volume to obtain the plant extract.
Adding 4.2 parts of thyme extract, 12.0 parts of rosemary extract, 10.0 parts of swertia japonica extract, 10.0 parts of arnebia euchroma extract, 7.0 parts of 2, 4-benzyl dichloroacrylate, 10.0 parts of sodium isostearoyl lactylate, 10.0 parts of sodium myristamide propyl PG-dimethyl ammonium chloride phosphate, 1.0 part of lactic acid and 35.8 parts of 1, 3-propylene glycol into a stirring tank according to the mass fraction ratio, and uniformly stirring and mixing at 300r/min to obtain the plant anti-dandruff and anti-itching composition.
Comparative example 6
Adding 4.2 parts of thyme extract, 12.0 parts of rosemary extract, 10.0 parts of swertia japonica extract, 10.0 parts of arnebia euchroma extract, 7.0 parts of 2, 4-benzyl dichloroacrylate, 10.0 parts of sodium isostearoyl lactylate, 10.0 parts of CAB-35 myristamidopropyl betaine, 1.0 part of lactic acid and 35.8 parts of 1, 3-propylene glycol into a stirring tank according to the mass fraction ratio, and uniformly stirring and mixing at 300r/min to obtain the plant anti-dandruff and anti-itching composition.
Wherein the preparation methods of the thyme extract, the rosemary extract, the swertia japonica extract, and the arnebia euchroma extract are the same as those of the above example 1.
Comparative example 7
Adding 4.2 parts of thyme extract, 12.0 parts of rosemary extract, 10.0 parts of swertia japonica extract, 10.0 parts of arnebia euchroma extract, 7.0 parts of 2, 4-benzyl dichloroacrylate, 10.0 parts of sodium isostearoyl lactylate, 10.0 parts of PEG-40 hydrogenated castor oil, 1.0 part of lactic acid and 35.8 parts of 1, 3-propylene glycol into a stirring tank according to the mass fraction ratio, and uniformly stirring and mixing at 300r/min to obtain the plant anti-dandruff and anti-itching composition.
Wherein the preparation method of the thyme extract, the rosemary extract, the swertia japonica extract, and the arnebia euchroma extract is the same as that of example 1.
Comparative example 8
Adding 4.2 parts of thyme extract, 12.0 parts of rosemary extract, 10.0 parts of swertia japonica extract, 10.0 parts of arnebia euchroma extract, 7.0 parts of 2, 4-benzyl dichloroacrylate, 10.0 parts of sodium isostearoyl lactylate, 10.0 parts of tween-80, 1.0 part of lactic acid and 35.8 parts of 1, 3-propylene glycol into a stirring tank according to the mass fraction ratio, and uniformly stirring and mixing at 300r/min to obtain the plant anti-dandruff and anti-itching-relieving composition.
Wherein the preparation methods of the thyme extract, the rosemary extract, the swertia japonica extract, and the arnebia euchroma extract are the same as those of the above example 1.
Comparative example 9
Adding 4.2 parts of thyme extract, 12.0 parts of rosemary extract, 10.0 parts of swertia japonica extract, 10.0 parts of arnebia euchroma extract, 7.0 parts of 2, 4-benzyl dichloroacrylate, 10.0 parts of sodium isostearoyl lactylate, 10.0 parts of fatty alcohol-polyoxyethylene ether sodium sulfate, 1.0 part of lactic acid and 35.8 parts of 1, 3-propylene glycol into a stirring tank according to the mass fraction ratio, and stirring and mixing uniformly at 300r/min to obtain the plant anti-dandruff and anti-itching composition.
Wherein the preparation method of the thyme extract, the rosemary extract, the swertia japonica extract, and the arnebia euchroma extract is the same as that of example 1.
Comparative example 10
Adding 4.2 parts of thyme extract, 12.0 parts of rosemary extract, 10.0 parts of swertia japonica extract, 10.0 parts of arnebia euchroma extract, 7.0 parts of 2, 4-benzyl dichloroacrylate, 10.0 parts of sodium isostearoyl lactylate, 10.0 parts of fatty alcohol ammonium sulfate, 1.0 part of lactic acid and 35.8 parts of 1, 3-propylene glycol into a stirring tank according to the mass fraction ratio, and uniformly stirring and mixing at 300r/min to obtain the plant anti-dandruff and anti-itching composition.
Wherein the preparation methods of the thyme extract, the rosemary extract, the swertia japonica extract, and the arnebia euchroma extract are the same as those of the above example 1.
Application example shampoo
The formula of the blank shampoo is as follows:
TABLE 4 formulation of blank shampoo
The preparation method of the blank shampoo comprises the following steps: firstly, sufficiently weighing the component of the phase A, sequentially adding the component of the phase A into a beaker, stirring at 80 ℃ until the components are uniformly dispersed, adding the phase B, uniformly stirring, adding the dispersed phases C and D, uniformly stirring, cooling to 50 ℃, sequentially adding the component of the phase E, and uniformly stirring to obtain the blank shampoo base material without the anti-dandruff agent.
The different addition amounts of the plant anti-dandruff and anti-itching composition prepared in example 1 are added into the formula of the blank shampoo to test the inhibition effect on malassezia, the results are shown in table 5, and the result shows that the plant anti-dandruff and anti-itching composition prepared in example 1 can enable the shampoo to have extremely strong malassezia inhibition effect by adding 0.5% of the plant anti-dandruff and anti-itching composition into the blank shampoo.
TABLE 5 Malassezia inhibition effect of the plant anti-dandruff antipruritic composition prepared in example 1 at various addition levels
The plant anti-dandruff and anti-itching compositions prepared in examples 1-5 and comparative examples 1-4 are respectively added into a blank shampoo formula according to the addition amount of 0.5%, the inhibition effect on malassezia is tested, the test mode is that the sample 1 is diluted, the action time is 5min, the action time is 10min, and the test results are shown in table 6.
TABLE 6 Malassezia inhibition effect of the plant anti-dandruff antipruritic compositions prepared in examples 1 to 5
The plant anti-dandruff and anti-itch composition prepared in example 1 and comparative example 5 was subjected to comparative test of anti-itch effect, the test method was as follows: the 3 rd 3cm by 3cm area of skin was randomly marked on the inside of the arm of healthy subjects as a blank, negative control and experimental group, respectively. The test area was treated by tearing with scotch tape (repeated 10 times), then a 3cm by 3cm nonwoven fabric completely soaked in 10mg/ml histamine solution was applied to the negative control and experimental group areas, and was peeled off after 10min, the experimental group was coated with an aqueous solution containing an anti-dandruff antipruritic agent after the skin solution had dried out, the negative control and blank groups were not treated, and the condition of the subjects was evaluated and registered, and the time at which the subjects no longer experienced itching was taken as the test result, see table 7.
The test results show that the itching relieving effect is obviously reduced when the process of extracting the filter residue without the fermentation extracting solution is adopted, which shows that the extract obtained by the secondary fermentation of the filter residue in the plant extraction process can provide effective itching relieving effect, and the method has obvious improvement compared with the conventional plant solvent extraction.
TABLE 7 antipruritic effect of the plant anti-dandruff and antipruritic compositions prepared in example 1 and comparative example 5
Based on the above experiments, the anti-itch effects of the plant anti-dandruff and anti-itch compositions prepared in examples 1 to 5 and comparative examples 1 to 4 were tested, the experimental procedures were as described above, and the results of the test at a concentration of 2.0% are shown in Table 8, and it can be seen from the experimental results that each plant component of the present invention provides an anti-itch effect, indicating that the more plant components the composition of the present invention contains, the better the anti-itch effect.
TABLE 8 antipruritic effects of the plant anti-dandruff antipruritic compositions prepared in examples 1 to 5 and comparative examples 1 to 4
The plant anti-dandruff and antipruritic compositions prepared in example 1 and comparative examples 6 to 10 were added to a blank shampoo to test the inhibitory effect of malassezia (test standard: GB/T15979). From the experimental results (table 9), it can be seen that the anti-dandruff and anti-itching agent 1 has the best inhibition effect on malassezia, is obviously superior to other compositions, and particularly, after being stored at high temperature for one month, the anti-dandruff and anti-itching agent 1 still has a very strong inhibition effect on malassezia, which shows that the myristamide PG-dimethyl ammonium chloride phosphate sodium has obvious stability and bacteriostasis synergy on the preparation.
TABLE 9 Malassezia inhibition effect of the plant anti-dandruff antipruritic compositions prepared in example 1 and comparative examples 6 to 10
Based on the requirements of new European Union regulations, ZPT can not be used as an antidandruff agent in shampoo, OCT (about 700 yuan/kg) is used as an antidandruff agent, the dosage is usually 0.5-0.7%, and the use cost is high, so OCT is selected as an experimental control, and the plant antidandruff and antipruritic composition prepared in example 1 is considered to inhibit and enhance malassezia in commercially available shampoo, so that the aim of reducing the use cost is achieved. The anti-dandruff effect was evaluated by the inhibition rate of malassezia (test standard: GB/T15979), and the test results are shown in Table 10.
TABLE 10 inhibitory Effect of OCT and the plant anti-dandruff antipruritic compositions obtained in example 1 on Malassezia in commercially available shampoos
From the experimental results in table 10, the dosage of the anti-dandruff agent in different formula systems is obviously different, and from the experimental data of shampoo nos. 02, 04 and 05, the anti-dandruff effect is obvious when 0.1% OCT is compounded with 0.5% plant anti-dandruff and anti-itching composition; the dandruff removing effect is tested by expanding the dilution ratio, the inhibition effect of the experimental scheme of the compound composition on malassezia is still effective, and the plant dandruff removing and itching relieving composition has an obvious effect on dandruff removal.
Based on the malassezia inhibition effect test of the plant anti-dandruff and anti-itching compositions prepared in example 1 and comparative examples 6 to 10, the compounded 0.5% plant anti-dandruff and anti-itching composition and shampoo 01 to 05 containing only 0.1% by weight of oct were separately dispensed in 10 parts, totaling 100 parts, and distributed to the test population (100 persons) for comparative use. Each person continuously uses the shampoo for 4 weeks, questionnaires are graded according to the use feelings of the testees, the grading is 1-10, the grade is the worst grade at 1, the grade is the best grade at 10, the higher the grade is, the better the dandruff removing and itching relieving effects of the product are, and the average evaluation result is shown in figure 3.
From the scoring result, the dandruff removing and itching relieving shampoo adopting the compound scheme obviously obtains the score better than the common shampoo, and the reason is that the plant extract contains the directly extracted active ingredients and the nutrient components obtained by fermentation, so that the scalp itching condition of a test user is greatly reduced, and the scalp itching condition is greatly reduced, and the malassezia is killed by the antibacterial components, and the scalp itching condition has good repairing effect on scalp hair roots.
The above examples are only intended to illustrate the detailed process of the present invention, and the present invention is not limited to the above detailed process, i.e., it is not intended that the present invention necessarily depends on the above detailed process for its implementation. It should be understood by those skilled in the art that any modifications to the present invention, equivalent substitutions of the raw materials of the product of the present invention, and the addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A preparation method of a plant anti-dandruff and anti-itching composition based on fermentation is characterized by comprising the following steps:
s10, respectively pretreating and sieving fresh thyme, rosemary, swertia japonica and arnebia euchroma to prepare powder;
s20, adding the powder into the extracting solution respectively for extraction, and filtering to obtain filtrate and filter residue;
s30, concentrating the filtrate after secondary filtration to obtain concentrated filtrate; uniformly mixing the filter residue with water, adding lactobacillus for fermentation, collecting supernatant, and concentrating to obtain filter residue fermentation liquor;
s40, mixing the concentrated filtrate with the filter residue fermentation liquor to respectively prepare a thyme extracting solution, a rosemary extracting solution, a Japanese swertia herb extracting solution and a Sinkiang arnebia root extracting solution, and mixing the thyme extracting solution, the rosemary extracting solution, the Japanese swertia herb extracting solution and the Sinkiang arnebia root extracting solution to prepare plant extracting solutions;
s50, uniformly mixing the plant extract, 2, 4-benzyl dichloroacrylate, sodium isostearoyl lactylate, sodium myristamidopropyl PG-dimethyl ammonium chloride phosphate, lactic acid and 1, 3-propylene glycol to prepare the anti-dandruff and itching-relieving composition.
2. The method for preparing an anti-dandruff and anti-itch composition based on fermented plants according to claim 1, wherein in step S50, the anti-dandruff and anti-itch composition is prepared using the following raw materials in parts by weight:
3. the method for preparing an anti-dandruff and anti-itch composition based on fermented plants according to claim 1, wherein in step S50, the anti-dandruff and anti-itch composition is prepared using the following raw materials in parts by weight:
and 10 parts of myristamidopropyl PG-dimethyl ammonium chloride sodium phosphate.
4. The method for preparing a composition for removing dandruff and relieving itching based on fermented plants according to claim 1, wherein the step S10 is specifically as follows: the method comprises the steps of drying fresh picked plants by hot air at 30-60 ℃, then crushing at-35-0 ℃, and sieving with a 300-mesh sieve to obtain plant powder.
5. The method for preparing a composition for removing dandruff and relieving itching based on fermented plants according to claim 1, wherein the step S20 is specifically: respectively transferring the plant powder to an extraction tank, selecting a mixed solution of 1, 3-propylene glycol and water with a volume ratio of (1-5) to (1-5) as an extracting solution, extracting for 2-5h at 50-80 ℃ at 200-500 r/min, and filtering and separating to respectively obtain filtrate and filter residue.
6. The method for preparing a composition for removing dandruff and relieving itching based on fermented plants according to claim 1, wherein in step S30: concentrating the filtrate to 1/2 of the original filtrate volume; mixing the filter residue with water according to a volume ratio of 1-1;
and (3) measuring the total ammonia content of the obtained fermentation filtrate, taking the content of more than 0.3 percent as a qualified judgment index of concentration, and further concentrating the obtained fermentation filtrate until the content requirement is met if the content requirement is not met.
7. The method for preparing a fermented-based plant anti-dandruff and anti-itch composition according to claim 6, wherein the Lactobacillus is LactobacillusMixed strain composed of Lactobacillus plantarum, lactobacillus rhamnosus, lactobacillus acidophilus and Bifidobacterium, and the concentration of Lactobacillus is 2 x 10 7 CUF/ml。
8. The method for preparing a plant anti-dandruff and anti-itch composition based on fermentation according to claim 1, wherein benzyl 2, 4-dichloroacrylate is prepared as follows:
adding 2, 4-dichlorobenzyl alcohol, dichloromethane and triethylamine into a three-neck flask provided with a condenser and a dropping funnel, starting mechanical stirring in an ice water bath, dropwise adding acryloyl chloride, continuing to react after the reaction is finished, filtering reaction liquid after the reaction is finished, extracting filtrate by using ethyl acetate, removing the ethyl acetate, and drying in a vacuum drying oven to obtain white powder solid, namely 2, 4-dichlorobenzyl acrylate;
wherein the molar ratio of the 2, 4-dichlorobenzyl alcohol to the acryloyl chloride to the triethylamine is 1.56.
9. A plant composition for removing dandruff and relieving itching, which is prepared by the preparation method of any one of claims 1 to 8.
10. Use of a plant anti-dandruff and anti-itch composition prepared by the preparation method of any one of claims 1 to 8 in a hair shampoo product.
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| KR20070070985A (en) * | 2005-12-29 | 2007-07-04 | 에스케이케미칼주식회사 | Sterilization composition and sterilization method using the same |
| WO2019040532A1 (en) * | 2017-08-21 | 2019-02-28 | Allele Biotechnology & Pharmaceuticals, Inc. | Light-absorbing compositions and methods of use |
| CN113398029A (en) * | 2021-07-08 | 2021-09-17 | 珠海博御中医药研究有限公司 | Antibacterial and anti-dandruff shampoo and preparation method thereof |
| CN113398036A (en) * | 2021-07-15 | 2021-09-17 | 忧立舒医药科技(广东)有限公司 | No-wash plant scalp hair cleaning agent and preparation method and application thereof |
| CN113817164A (en) * | 2020-06-12 | 2021-12-21 | 北京化工大学 | Hypoxic sensitive drug carrier polymer and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20070070985A (en) * | 2005-12-29 | 2007-07-04 | 에스케이케미칼주식회사 | Sterilization composition and sterilization method using the same |
| WO2019040532A1 (en) * | 2017-08-21 | 2019-02-28 | Allele Biotechnology & Pharmaceuticals, Inc. | Light-absorbing compositions and methods of use |
| CN113817164A (en) * | 2020-06-12 | 2021-12-21 | 北京化工大学 | Hypoxic sensitive drug carrier polymer and preparation method and application thereof |
| CN113398029A (en) * | 2021-07-08 | 2021-09-17 | 珠海博御中医药研究有限公司 | Antibacterial and anti-dandruff shampoo and preparation method thereof |
| CN113398036A (en) * | 2021-07-15 | 2021-09-17 | 忧立舒医药科技(广东)有限公司 | No-wash plant scalp hair cleaning agent and preparation method and application thereof |
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