Polymorphic zinc and organic acid composition for targeted scalp barrier repair as well as preparation method and application of polymorphic zinc and organic acid composition

Abstract

The invention provides a polymorphic zinc and organic acid composition for targeted scalp barrier repair as well as a preparation method and application of the polymorphic zinc and organic acid composition. The composition is prepared from the following components in percentage by mass: 1 to 80 percent of yeast / zinc fermentation product, 1 to 20 percent of polyaspartic acid chelated zinc, 0.5 to 20 percent of gluconolactone, 0.5 to 6 percent of hydroxydecanoic acid, 1 to 10 percent of succinyl glycan and the balance of water or other pharmaceutically / cosmetically acceptable carriers. Wherein the mass ratio of the yeast / zinc fermentation product to the polyaspartic acid chelated zinc is (1: 1)-(8: 1); the mass ratio of the hydroxydecanoic acid to the gluconolactone is (1: 0.5)-(1: 3). The invention provides an efficient, mild and multi-effect synergistic nursing composition, and the composition realizes a three-in-one scalp regulation mechanism of barrier repair, mild bacteriostasis and long-acting moisturizing through unique component synergy.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of daily chemicals, in particular to the technology of head skin care in the field of skin care, and especially to a multi-form zinc and organic acid composition targeting scalp barrier repair, a preparation method thereof and application thereof in head washing and care products. BACKGROUND

[0002] A healthy scalp relies on the synergistic effect of physical barrier, microecological barrier and chemical barrier to maintain environmental stability. The physical barrier is composed of keratinocytes and intercellular lipids, forming a dense "brick wall structure", effectively locking water and resisting the invasion of external pollutants and microorganisms. The microecological barrier is composed of a complex community of symbiotic microorganisms on the scalp surface, in which beneficial bacteria dominate, inhibit the excessive proliferation of harmful bacteria by secreting antibacterial peptides, and maintain bacterial diversity. The chemical barrier is composed of weakly acidic sebum film and natural antibacterial ingredients, and its slightly acidic environment inhibits the growth of pathogenic bacteria, activates epidermal enzyme activity and promotes barrier repair. Therefore, the integrity of the scalp barrier function is crucial to maintain the health of the scalp and hair.

[0003] However, existing scalp care products focus on a single function, such as strong cleaning of oil, dandruff removal or oil control, and generally have the following defects:

[0004] Insufficient barrier repair or complex ingredients: excessive cleaning or strong dandruff-removing ingredients (such as high-concentration sulfate surfactants, zinc pyrithione) can easily damage the sebum film and intercellular lipids, leading to damage to the physical barrier and causing or exacerbating dryness, tightness, itching, desquamation and even inflammatory reactions on the scalp (such as recurrent episodes of sensitive scalp and seborrheic dermatitis). Single moisturizing ingredients (such as ceramides, glycerol or extracts) can alleviate dryness, but have limited effects on microecological regulation.

[0005] Single efficacy and lack of long-term effectiveness: traditional antibacterial dandruff-removing ingredients (such as zinc pyrithione and ketoconazole) can inhibit Malassezia, but long-term use can cause dryness of the scalp, broad-spectrum antibacterial ingredients indiscriminately kill beneficial bacteria, and have limited effects on promoting beneficial bacteria and maintaining overall microecological balance; single oil control ingredients are difficult to achieve long-term moisturizing and dandruff removal. There is a lack of multifunctional solutions that can effectively repair the barrier, inhibit harmful bacteria and achieve long-term oil control and dandruff removal.

[0006] "Stimulation and efficacy" contradiction: some products use highly irritating ingredients (such as salicylic acid and acidic exfoliating agents) to pursue immediate efficacy, although they have certain exfoliating or oil control effects, they further weaken the barrier function, forming a vicious cycle.

[0007] Low utilization efficiency of zinc: traditional zinc salts (such as zinc sulfate and zinc carbonate) have low bioavailability, are difficult to effectively penetrate the stratum corneum to reach the action site, and free zinc ions are easily combined with anions in the scalp environment to precipitate and lose activity.

[0008] In summary, the current scalp care technology is faced with three core problems of "stimulation and efficacy" contradiction, single function and long-acting deficiency. It is urgent to develop a multifunctional composition which can synergistically repair scalp barrier, mildly inhibit bacteria, long-acting moisturize and effectively control oil and dandruff, and has low irritation. SUMMARY

[0009] In order to overcome the deficiencies of the prior art, the purpose of the present application is to provide a high-efficiency, mild and multi-effect care composition for repairing scalp barrier function. The composition realizes the trinity scalp regulation mechanism of "barrier repair, mild bacteria inhibition and long-acting moisturization" through the synergy of unique components.

[0010] Another purpose of the present application is to provide a preparation method of the above-mentioned multi-form zinc and organic acid composition targeting scalp barrier repair.

[0011] Still another purpose of the present application is to provide the application of the above-mentioned multi-form zinc and organic acid composition targeting scalp barrier repair in the preparation of head washing and care products.

[0012] The technical solution to achieve the first purpose is as follows:

[0013] A multi-form zinc and organic acid composition targeting scalp barrier repair, the composition comprises (or consists of) the following components: yeast / zinc fermentation product, polyaspartic acid chelated zinc, gluconolactone, hydroxydecanoic acid and succinyl polysaccharide.

[0014] Preferably, the composition comprises the following components by total mass percentage of the composition:

[0015] Yeast / zinc fermentation product 1-80%, polyaspartic acid chelated zinc 1-20%, gluconolactone 0.5-20%, hydroxydecanoic acid 0.5-6%, succinyl polysaccharide 1-10%, and the balance is water or other pharmaceutically / cosmetically acceptable carriers. The mass ratio of yeast / zinc fermentation product to polyaspartic acid chelated zinc is (1:1)-(8:1); the mass ratio of hydroxydecanoic acid to gluconolactone is (1:0.5)-(1:3).

[0016] More preferably, the composition comprises the following components by total mass percentage of the composition:

[0017] Yeast / zinc fermentation product 20-80%, polyaspartic acid chelated zinc 1-20%, gluconolactone 1-10%, hydroxydecanoic acid 1-5%, succinyl polysaccharide 1-5%, and the balance is water or other pharmaceutically / cosmetically acceptable carriers. The mass ratio of yeast / zinc fermentation product to polyaspartic acid chelated zinc is (2.5:1)-(5:1); the mass ratio of hydroxydecanoic acid to gluconolactone is (1:0.7)-(1:3).

[0018] More preferably, the composition comprises the following components by total mass percentage of the composition:

[0019] Saccharomyces cerevisiae / zinc fermentation product 20-60%, polyaspartic acid chelated zinc 5-15%, gluconolactone 1.5-6%, hydroxydecanoic acid 2-4%, succinoglycan 2-4%, the balance being water or other pharmaceutically / cosmetically acceptable carriers. The mass ratio of the Saccharomyces cerevisiae / zinc fermentation product to the polyaspartic acid chelated zinc is (2.5:1)-(5:1); the mass ratio of the hydroxydecanoic acid to the gluconolactone is (1:0.75)-(1:3).

[0020] The Saccharomyces cerevisiae / zinc fermentation product is obtained by the following method:

[0021] The Saccharomyces cerevisiae / zinc fermentation product is obtained by the following method:

[0022] The specific steps are as follows:

[0023] The Saccharomyces cerevisiae / zinc fermentation product is obtained by the following method:

[0024] The Saccharomyces cerevisiae / zinc fermentation product is obtained by the following method:

[0025] Further, the strict sterilization temperature is 125℃; the added amount of the yeast strain is 0.5%; the initial stage maintains a low zinc concentration of 60mg / L ZnSO4; the zinc concentration of the fermentation liquor is gradually increased by 40mg / L each time; the temperature of the culture fermentation is 75℃, and the time is 12 hours; the enzymolysis reaction time is 24 hours; the heat reaction temperature is 105℃, and the treatment time is 4 hours; and the ultrafiltration membrane is selected to be <500KD.

[0026] The total zinc content in the polyaspartate chelated zinc is 400-800mg / kg, preferably 450-650mg / kg; and the weight average molecular weight (Mw) of the polymer is 10000-50000Da, preferably 20000-35000Da.

[0027] The succinyl polysaccharide is a polysaccharide compound, which is a linear polysaccharide connected by a plurality of glucose units through a glycosidic bond, and has a succinyl group (-CO-CH2-CH2-COO-) connected to the glucose unit, and the weight average molecular weight is 1.5×10 6 Da to 3.5×10 6 Da, preferably 2.0×10 6 Da to 3.0×10 6 Da.

[0028] The technical scheme for realizing the second object of the present application is as follows:

[0029] A preparation method of a multi-form zinc and organic acid composition for targeting scalp barrier repair, comprising the following steps:

[0030] 1. Add the formula amount of water and succinyl polysaccharide into a reaction container, and perform high-speed homogenization dispersion at a rotation speed of 2000-3000rpm.

[0031] 2. Warm up to 80-85℃, and maintain and stir at a stirring rotation speed of 200-500rpm for 20-30 minutes, so that the succinyl polysaccharide is completely dissolved and uniform.

[0032] 3. Cool the solution obtained in step 2 to 40-45℃.

[0033] 4. Add the formula amount of yeast / zinc fermentation product, polyaspartate chelated zinc, gluconolactone and hydroxydecanoic acid into the cooled solution in sequence, and stir uniformly at a stirring rotation speed of 200-500rpm.

[0034] 5. Cool the mixed solution obtained in step 4 to 37-39℃. Filter the product through a filter screen with a suitable mesh number (such as 100-200 mesh) to obtain the multi-form zinc and organic acid composition for targeting scalp barrier repair.

[0035] Further, after step 4 or step 5, a pH regulator (such as citric acid, sodium citrate, lactic acid, sodium hydroxide, etc.) is used to adjust the pH of the care composition to 4.0-5.5.

[0036] The technical scheme for achieving the third object of the present application is as follows:

[0037] The application of the above-mentioned multi-modal zinc and organic acid composition targeting scalp barrier repair in the preparation of head care products.

[0038] Further, the head care product is selected from one or more of shampoo, hair rinse, hair conditioner, scalp serum, scalp gel, and scalp spray.

[0039] Further, the composition is added to the head care product in a low-temperature manner. More preferably, the addition temperature is 10-45°C, and most preferably, the addition temperature is room temperature.

[0040] Further, the head care product is a shampoo.

[0041] The shampoo comprises the following components by weight percentage:

[0042] Phase A: water balance, guar gum hydroxypropyltrimonium chloride small molecular weight 0.2%, guar gum hydroxypropyltrimonium chloride large molecular weight 0.1%, citric acid 0.05%;

[0043] Phase B: cocamidopropyl betaine 6%, sodium laureth sulfate 15%, lauryl hydroxysultaine 6%, cocamide 0.3%, ethylene glycol distearate 0.8%, cetearyl alcohol 0.2%, hydrogenated castor oil 0.2%;

[0044] Phase C: emulsified silicone oil 1785 POE 1.5%, emulsified silicone oil 7137 POE 1.2%, phenoxyethanol 0.4%, sodium benzoate 0.4%, glycerol 1.5%, fragrance 0.5%, sodium chloride 0.8%;

[0045] Phase D: the multi-modal zinc and organic acid composition targeting scalp barrier repair 4%;

[0046] The preparation process of the shampoo comprises the following steps:

[0047] At room temperature, the A phase raw materials are added into the emulsifying kettle while homogenizing, the homogenizing speed is 2500 RPM / min, homogenizing for 5 minutes, the stirring is started, the rotating speed is 300 RPM / min, the steam is started to heat to 90℃, the B phase raw materials are added, and homogenizing for 30 minutes; the condensate water is started to cool to 50-55℃, and homogenizing for 30 minutes, and then the temperature is continuously cooled to 40℃, the C phase raw materials and the D phase raw materials are added, and homogenizing for 20 minutes until uniform, and then the temperature is cooled to 38℃; after the inspection is qualified, the material is filtered out, and is canned.

[0048] By the above technical scheme, the application has the following beneficial technical effects:

[0049] 1) The composition of the application has the synergistic effect of the unique five core components, simultaneously repairing the physical barrier (moisturizing, enhancing defense), mildly inhibiting bacteria (inhibiting harmful bacteria, mild and non-irritating), maintaining the chemical barrier (weak acidic environment), and effectively controlling oil and dandruff;

[0050] 2) The composition of the application can be conveniently added into various head washing and protecting product formulas such as shampoo, essence, spray, jelly, etc. at low temperature (10-45℃, preferably room temperature), the process is simple, has no adverse effect on the physical and chemical properties of the product, and has good stability. BRIEF DESCRIPTION OF DRAWINGS

[0051] Figure 1 Schematic diagram of oil film for SZ95 cells using application examples 1, 2 and application comparative examples 1, 2;

[0052] Figure 2 Schematic diagram of oil film for SZ95 cells using application examples 4, 5 and application comparative examples 4, 5;

[0053] Figure 3 Schematic diagram of scalp oil improvement state using application example 1;

[0054] Figure 4 Schematic diagram of scalp oil improvement state using application example 4;

[0055] Figure 5 Schematic diagram of scalp oil improvement state using application example 6;

[0056] Figure 6 Schematic diagram of scalp dandruff state using application example 1;

[0057] Figure 7 Schematic diagram of scalp dandruff state using application example 5;

[0058] Figure 8 Schematic diagram of scalp dandruff state using application example 6. DETAILED DESCRIPTION

[0059] The following detailed description of specific embodiments of the application is presented for the purpose of illustration and description. It is not intended to be a limitation on the application. Unless otherwise indicated, the percentages in the examples are by weight percent (wt%), and the units of parts can be g or kg. Unless otherwise specified, the experimental methods were performed according to conventional conditions or the conditions recommended by the manufacturer.

[0060] The present application discloses a kind of high efficiency, mild, multi-effect synergy composition of multi-form zinc and organic acid for targeting scalp barrier repair.The composition comprises the following components by total mass percentage of the composition:

[0061] Yeast / zinc fermentation product 1-80%, polyaspartic acid chelated zinc 1-20%, gluconolactone 0.5-20%, hydroxydecanoic acid 0.5-6%, succinyl polysaccharide 1-10%, and the balance is water or other pharmaceutically / cosmetically acceptable carriers.The mass ratio of yeast / zinc fermentation product to polyaspartic acid chelated zinc is (1:1)-(8:1);The mass ratio of hydroxydecanoic acid to gluconolactone is (1:0.5)-(1:3).

[0062] Specifically comprising the following key components and their effects:

[0063] The yeast / zinc fermentation product is obtained by cyclic stress fermentation of a specific cold-tolerant Saccharomyces cerevisiae strain and zinc sulfate, which utilizes the bioaccumulation and transformation ability of yeast to convert zinc sulfate into small molecular weight, high bioavailability organic chelated zinc (such as zinc-polypeptide / amino acid complex).This product not only provides slow-release zinc ions, but also is rich in polysaccharides, amino acids and other prebiotic substances produced by yeast metabolism, which can activate keratinocyte receptors, promote targeted delivery of zinc, and nourish beneficial bacteria.

[0064] The yeast / zinc fermentation product is obtained by the following method:

[0065] The cold-tolerant Saccharomyces cerevisiae strain CGMCC No.15873 is used for cyclic stress stimulation fermentation with zinc sulfate, which utilizes the bioaccumulation ability of the yeast strain to zinc, combined with bioenzymatic technology for extraction and refinement of the fermentation product.The total zinc content in the obtained fermentation product is 20-100 mg / kg, preferably 60-80 mg / kg.

[0066] The specific steps are as follows:

[0067] The natural sugar cane molasses purified as a carbon source, zinc sulfate as a zinc source, after strict sterilization, the activation of the extremely cold tolerant Saccharomyces cerevisiae strain CGMCC No. 15873 (a commercially available product) is inoculated, the zinc sulfate is added, and the dynamic gradient zinc concentration cycle stress stimulation fermentation is carried out, the gradient increasing zinc stress based on the real-time biosensor feedback is adopted, the zinc ion selective electrode or the intracellular zinc concentration biosensor based on the fluorescent protein is integrated in the fermentation tank, the extracellular / intracellular zinc level is monitored in real time, the low zinc concentration 50-100 mg / L ZnSO4 is maintained in the initial stage, the zinc concentration of the fermentation broth is increased by a small gradient according to the sensor feedback yeast growth rate, intracellular zinc accumulation rate and metabolic activity parameters, the zinc concentration is increased by 20-50 mg / L ZnSO4 each time, when the growth rate is detected to be significantly reduced or the accumulation rate is detected to be on a platform, the zinc concentration is increased or the zinc concentration is temporarily reduced, the fermentation is carried out at 70-80 DEG C for 10-15 hours, the protease enzymolysis reaction is selected for 20-30 hours, the heat reaction is treated at 100-120 DEG C for 2-5 hours, the low-temperature centrifugation is carried out immediately after the enzymolysis, the ultrafiltration membrane is used for separation, the zinc-rich soluble component is quickly separated, and the supernatant is collected to obtain the yeast bacteria / zinc fermentation product.

[0068] Further, the strict sterilization temperature is 125 DEG C, the addition amount of the yeast strain is 0.5%, the low zinc concentration 60 mg / L ZnSO4 is maintained in the initial stage, the zinc concentration of the fermentation broth is increased by a small gradient, and the zinc concentration is increased by 40 mg / L each time, the fermentation temperature is 75 DEG C, and the fermentation time is 12 hours, the enzymolysis reaction time is 24 hours, the heat reaction temperature is 105 DEG C, and the treatment time is 4 hours, and the ultrafiltration membrane is selected to be <500KD.

[0069] The polyaspartic acid chelated zinc is high-molecular polymer chelated zinc, the polyaspartic acid chain is formed into a stable coordination bond with zinc ions through a plurality of carboxylic acid groups, the stability and water solubility of zinc are significantly improved, and precipitation inactivation with acid radical ions is avoided. The hydrophilic-lipophilic balance structure enhances the transdermal absorption of zinc, effectively supplements the zinc content in the deep layer of the epidermis, and cooperates with the fermentation product to realize the delivery of zinc from the shallow layer to the deep layer. The raw material of the application is purchased from Guangzhou Yuren Biotechnology Co., Ltd., and the commodity name is: aspartic zinc, which can be replaced by equivalent products, and is not limited to the application.

[0070] The polyaspartic acid chelated zinc is zinc ion (Zn 2+) and amide groups (-CONH-) on the polyaspartic acid chain, the active zinc element is precisely embedded in the long chain structure of polyaspartic acid to form a stable "zinc pool", which combines the natural moisturizing properties of polyaspartic acid and the biological function of zinc element; the total zinc content in polyaspartic acid chelated zinc is 400-800 mg / kg, preferably 450-650 mg / kg; the weight average molecular weight (Mw) of the polymer is 10000-50000 Da, preferably 20000-35000 Da.

[0071] Glucolactone is a natural organic compound derived from glucose oxidation. It is a cyclic lactone formed by the dehydration condensation of carboxyl (-COOH) and intramolecular hydroxyl after the oxidation of aldehyde group (-CHO) in glucose molecule. As a mild keratin renewal regulator and pH regulator, it regulates keratinocyte differentiation by chelating calcium ions, promotes the natural shedding of old keratin, and avoids excessive exfoliation damage to the barrier. At the same time, it will slowly hydrolyze into gluconic acid, maintaining a weakly acidic environment on the scalp, which is conducive to the stability of the chemical barrier and the growth of beneficial bacteria. It is more mild than salicylic acid, mandelic acid, etc. The raw material of the invention is purchased from Guangzhou Saifu Chemical Co., Ltd., with the trade name Univig GDL A20, and can be replaced by equivalent products, which is not a limitation of the invention.

[0072] Hydroxydecanoic acid is a class of ten-carbon fatty acids containing hydroxyl groups. According to the position of the hydroxyl group (-OH) on the carbon chain, there are many isomers (such as α-, β-, ω-hydroxydecanoic acid). In the field of cosmetics and medicine, α-hydroxydecanoic acid and ω-hydroxydecanoic acid have the most application value. The amphiphilic structure of hydroxydecanoic acid penetrates the stratum corneum and can effectively inhibit the reproduction of harmful bacteria such as Malassezia and Staphylococcus aureus by destroying the integrity of the cell membrane, reducing the causes of dandruff generation. At the same time, it can down-regulate the expression of sebaceous gland cell fatty acid synthase, reduce the synthesis of triglycerides, and thus reduce the secretion of oil. Its fatty acid structure also helps to improve the overall permeability of the composition. The raw material of the invention is purchased from Beijing Dongfangmiosen Biological Technology Co., Ltd., with the trade name SebumBate, and can be replaced by equivalent products, which is not a limitation of the invention.

[0073] Succinyl polysaccharide is a high molecular weight linear polysaccharide with succinyl groups attached to its glucose units. It can form a three-dimensional network structure of breathable hydration film on the scalp surface through intermolecular hydrogen bonds, significantly reducing transdermal water loss, and has long-lasting moisturizing ability comparable to hyaluronic acid, especially suitable for dry dandruff or barrier damaged scalp. At the same time, as a prebiotic, it can be selectively metabolized by specific beneficial bacteria (such as Staphylococcus epidermidis), promoting the colonization and proliferation of beneficial bacteria and regulating the microecological balance. The raw material of the invention is purchased from Nanjing Gutian Chemical Co., Ltd., with the trade name: SH, which can be replaced by equivalent products, which is not a limitation of the invention.

[0074] Succinoglycan is a polysaccharide compound, which is a linear polysaccharide formed by a plurality of glucose units connected by glycosidic bonds, and has succinyl groups (-CO-CH2-CH2-COO-) connected to the glucose units, and has a weight average molecular weight of 1.5 x 10 6 Da to 3.5 x 10 6 Da, preferably 2.0 x 10 6 Da to 3.0 x 10 6 Da.

[0075] The design principle of the multi-morphology zinc and organic acid composition formula targeting scalp barrier repair is briefly described as follows:

[0076] The present application innovatively designs from the three dimensions of "zinc supplementation, zinc stabilization, and prebiotics" to address the challenges of scalp barrier repair: the use of yeast fermentation to convert inorganic zinc into easily absorbed organic chelated zinc (small molecules), combined with high molecular weight polyaspartic acid chelated zinc (stable and good transdermal), to construct a dual-channel zinc delivery system, significantly improve the bioavailability of zinc, and directly reach the deep layer of the hair follicle to achieve efficient zinc supplementation. The prebiotics (polysaccharides, amino acids) and succinoglycan in the fermentation products nourish the scalp and repair the scalp barrier; hydroxyl capric acid precisely targets and inhibits harmful bacteria such as Malassezia; gently updates the keratin (gluconolactone), provides long-lasting moisture retention (succinoglycan), and enhances the physical barrier defense capability, with hydroxyl capric acid synergistically controlling oil. The components work together closely to ultimately achieve integrated regulation of "barrier repair, mild bacteria inhibition, and long-lasting moisture retention".

[0077] Efficient zinc utilization and delivery: through the "yeast fermentation organic zinc + high molecular weight chelated zinc" dual-zinc system, the bioavailability and transdermal absorption rate of zinc are significantly improved, effective zinc supplementation and stabilization from the superficial to the deep layer of the scalp are achieved, and the problem of low utilization rate of traditional zinc salts is solved. Gluconolactone gently regulates keratin, hydroxyl capric acid precisely inhibits bacteria, and the overall pH of the composition is adapted to the scalp environment, which can effectively reduce the irritation of surfactants and relieve scalp itching. It is friendly to sensitive scalp and seborrheic dermatitis populations, and has no damage to the hair. Succinoglycan provides excellent long-lasting moisture retention; hydroxyl capric acid and zinc ions synergistically regulate sebum secretion to achieve source oil control.

[0078] Examples 1-6 and Comparative Examples 1-5

[0079] The composition formula ingredient table of the present application examples 1-6 is shown in Table 1 below.

[0080] Table 1 Composition formula of examples 1-6 (weight percentage %)

[0081] Component Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Water 25％ 37％ 35％ 29％ 68％ 27％ Succinoglycan \ 4％ 2％ 2％ 1.5％ 4％ Yeast / Zinc Fermentation Product 60％ 40％ 40％ 50％ 22％ 50％ Polyaspartate Chelated Zinc 15％ 15％ 15％ 15％ 5％ 10％ Gluconolactone \ 2％ 6％ 2％ 1.5％ 5％ Hydroxydecanoic Acid \ 2％ 2％ 2％ 2％ 4％ pH Adjuster q.s. q.s. q.s. q.s. q.s. q.s.

[0082] Example 1 is a simplified formulation example containing only the core zinc delivery components (fermentation product + chelated zinc) and water, more preferred formulations such as Examples 2-6 contain all five components.

[0083] Comparative Examples 1-3 are not prepared as separate compositions, but rather the control materials are added directly into a shampoo base formulation (see Shampoo Applications section below).

[0084] Comparative Example 4: does not contain the yeast / zinc fermentation product compared to Example 4.

[0085] Comparative Example 5: contains significantly lower levels of each active ingredient (below the lower end of the preferred ranges) compared to Examples 5 / 6, such as 18% yeast / zinc fermentation product, 0.8% polyaspartic acid chelated zinc, 0.8% gluconolactone, 0.5% hydroxycapric acid, 0.4% succinoglycan.

[0086] Preparation Method:

[0087] Example 1:

[0088] The preparation method comprises the following steps:

[0089] The water is added to a jacketed mixing kettle, the yeast / zinc fermentation product and the polyaspartic acid chelated zinc are added, and the mixture is stirred at room temperature at a stirring speed of 300 rpm for 20 minutes. The pH of the mixture is adjusted to 4.5 using a pH adjuster to obtain the care composition.

[0090] Examples 2-6 and Comparative Examples 4-5:

[0091] The preparation method comprises the following steps:

[0092] The formula amount of water and succinoglycan are added to a jacketed mixing kettle, and high-speed homogenization dispersion is performed at a speed of 2500 rpm, the temperature is raised to 82°C, and the succinoglycan is completely dissolved and uniformly dispersed by stirring at a stirring speed of 300 rpm for 25 minutes. The solution is cooled to 41°C, and the formula amount of yeast / zinc fermentation product, polyaspartic acid chelated zinc, gluconolactone and hydroxycapric acid are sequentially added, and the mixture is stirred at a stirring speed of 300 rpm to obtain the care composition.

[0093] Application Examples and Application Comparative Examples

[0094] The following examples and comparative examples are applied in shampoo formulations, and the specific component weights and preparation methods are as follows (Table 2).

[0095] Table 2 Shampoo Formulation (weight percent %) for Examples and Comparative Examples

[0096]

[0097] Preparation process of shampoo: clean and sterilize the equipment, and then wait for use; at room temperature, add the raw materials of phase A into the emulsifying kettle while homogenizing (homogenization speed: 2500 RPM / min), homogenize for 5 minutes, start stirring (speed: 300 RPM / min), start steam heating to 90°C, add the raw materials of phase B, and homogenize for 30 minutes; start condensate water to cool to 50-55°C, and homogenize for 30 minutes, continue to cool to 40°C, add the raw materials of phase C and phase D, and homogenize for 20 minutes until uniform, then cool to 38°C; after inspection, filter the product with 100 mesh sterilized filter cloth, and then bottle.

[0098] Application Comparative Example 1: phase D is zinc sulfate 0.3% + pyrithione zinc 0.3% (directly added, not in the form of composition)

[0099] Application Comparative Example 2: phase D is sodium hyaluronate 0.2% + glycerol 2% + ceramide 0.2% (directly added, not in the form of composition)

[0100] Application Comparative Example 3: phase D is salicylic acid 0.3% + glycolic acid 0.3% (directly added, not in the form of composition)

[0101] Application Comparative Example 4: phase D is the composition corresponding to Example 4 (but does not contain yeast / zinc fermentation product), and the composition is added in an amount of 4%.

[0102] Application Comparative Example 5: phase D is the composition corresponding to Example 5 (the composition content is lower than the preferred scheme), and the composition is added in an amount of 4%.

[0103] The following is the content of the efficacy test example of the composition of the application.

[0104] I. Balancing the flora and inhibiting Malassezia experiment

[0105] Research shows that Malassezia is an important factor for dandruff formation and aggravation. Malassezia can secrete lipase to decompose triglyceride and saturated fatty acid in sebum into unsaturated fatty acids such as arachidonic acid and oleic acid. These metabolites change the pH of the scalp and affect the integrity of the scalp, weaken the epidermal barrier function, cause immune stimulation, and then induce inflammatory response, cause keratinocytes to produce inflammatory cytokines such as IL-1, IL-6 and TNF-α, induce skin inflammation, itching and epidermal cell hyperplasia, and ultimately cause dandruff. By evaluating whether the composition can effectively balance and inhibit the activity of Malassezia, reduce the secretion of lipase, and protect the scalp barrier, the effect of anti-dandruff can be achieved.

[0106] Reference QB-T2738-2012 "Evaluation of antibacterial and bacteriostatic effect of daily chemical products" Part VII-7.3 Test method for bacteriostatic effect of bacteriostatic daily chemical products (suspension quantitative method), the test strain selected is Mslassezia Furfur ATCC 44344.

[0107] Specific operation steps: take the test bacteria 24h fresh slant culture with PBS, dilute to 5.0×10 5 CFU / mL~4.5×10 6 CFU / mL bacteria suspension for standby. Take sterile test tube, first add 5.0mL sample, place in 20℃±1℃ water bath for 5min, then add 0.1mL test bacteria suspension, mix quickly and immediately start timing. Take 1.0mL test bacteria and sample mixture to inoculate 2 plates, pour culture medium. When the bacteria amount cannot be counted, dilute 10 times in series with PBS, select appropriate dilution to take 1.0mL to inoculate 2 plates, and count the viable bacteria. At the same time, use PBS instead of sample to carry out parallel test as positive control. The positive control recovery bacteria colony count is between 1.0×10 4 CFU / mL~9.0×10 4 CFU / mL. Take the same batch of PBS and culture medium as negative control. All test samples and control samples are cultured at 36℃±1℃, and the bacterial proliferative culture is observed for 48h to observe the final results; the test is repeated 3 times, and the bacteriostatic rate is calculated.

[0108]

[0109] In the formula: A 对照 : indicates the positive control group recovery bacteria amount, unit: CFU / mL;

[0110] A 样品 : indicates the recovery bacteria amount of the sample group, unit: CFU / mL.

[0111] The test results represent the bacteriostatic rate of the sample on Malassezia. When the bacteriostatic rate is ≥50%-90%, it is judged to have bacteriostatic effect; when the bacteriostatic rate is ≥90%, it is judged to have strong bacteriostatic effect, indicating that the sample has anti-dandruff effect. Test results (as shown in Table 3).

[0112] Table 3 Bacteriostatic effect test results

[0113]

[0114] From the test data of Table 3, it can be seen that the shampoo containing the composition of the present application (Examples 1-6) exhibits significant inhibition effect on Malassezia (bacteriostatic rate > 70%), which is much better than each of the comparative examples. The excellent bacteriostatic effect of Examples 6, 3 and 4 is due to the combination of the double zinc system and the organic acid combination to achieve the inhibition of harmful microorganisms. On the one hand, the organic acid combination can improve the permeability of the composition to the skin and enhance the utilization rate of the composition, and the hydroxyl structure of the acid raw material can change the permeability of the microbial cell membrane, leading to the leakage of cell contents to achieve the bacteriostatic effect. On the other hand, zinc ions can bind to bacterial cell membranes and membrane proteins, destroy their structure, enter the cell and destroy the enzymes of the electron transport system and react with DNA to achieve the bacteriostatic effect.

[0115] The effect of Example 1 is significantly better than Comparative Example 1 using only traditional zinc salt, which proves the superiority of the double zinc system (yeast / zinc fermentation product + polyaspartic acid chelated zinc) in inhibiting harmful bacteria. The comparison between Example 4 and Comparative Example 4 clearly shows the key contribution of yeast / zinc fermentation product to improving the bacteriostatic effect. The comparison between Examples 5 / 6 and Comparative Example 5 shows that the synergistic effect of each active ingredient within the preferred content range is essential to achieve high-efficiency bacteriostasis. The composition of the present application has good anti-dandruff potential by effectively inhibiting Malassezia.

[0116] II. Oil secretion inhibition experiment

[0117] Sebum is the main component of the lipid film on the surface of the skin, which is secreted by sebaceous glands. Abnormal secretion of sebaceous glands and lipid peroxidation are considered to be the main factors causing problems in oily skin. Therefore, the key to regulating oily skin is to inhibit the excessive secretion of sebaceous glands, improve the quality of sebum, and reduce the occurrence of lipid peroxidation. By constructing a cell lipid overexpression model, the effect of the sample on the lipid expression of human sebaceous cells is explored, so as to evaluate the oil control effect of the sample.

[0118] The test is designed according to "Linoleic Acid Induced Changes in SZ95 Sebocytes—Comparison with Palmitic Acid and Arachidonic Acid".

[0119] The cells used for testing are human sebaceous cells (SZ95).

[0120] Specific operation steps: First, the cryopreserved SZ95 human sebaceous gland cells were recovered, inoculated into culture bottles, and expanded in DMEM medium without sodium pyruvate at 37°C in a 5% CO2 incubator. After the cells entered the logarithmic growth phase, they were washed twice with PBS, trypsinized, centrifuged to remove the supernatant, resuspended, and inoculated into culture dishes containing coverslips (2 mL of cell suspension per well), and continued to be cultured until the confluence reached 50%. The model control group was replaced with medium containing linoleic acid and 10% fetal bovine serum, and the sample group was added with a certain concentration of application examples or application comparative examples mixed with linoleic acid, and continued to be cultured for 72 hours. After the treatment was completed, the medium was discarded, the cells were fixed with 4% paraformaldehyde for 15 minutes, DAPI was used to stain the cell nucleus, Nile red was used to stain the lipid, and after overnight sealing, the fluorescence microscope was observed and the image was taken.

[0121] Data were analyzed using GraphPad Prism 8.0, expressed as mean ± standard error, and compared between groups by t-test or one-way ANOVA. The criterion for judging whether the sample group significantly reduced the relative expression rate of oil compared with the model control group (p<0.05) was used to verify the oil control effect of the sample. Linoleic acid was used to construct the lipid overexpression model throughout the experiment, combined with fluorescence staining and quantitative analysis, to systematically evaluate the inhibitory effect of the examples or comparative examples on the synthesis of sebaceous gland cells.

[0122] The lipid expression of SZ95 cells in the sample group was reduced compared with the model control group, and the result *p<0.05, the difference was significant, indicating that the sample had the effect of reducing the lipid expression of SZ95 cells at this concentration. See the staining Figures 1-2 test results (as shown in Table 4).

[0123] Table 4 Staining test results

[0124]

[0125]

[0126] Note: The oil expression rate of the model control group is set to 100%. All sample groups showed statistically significant differences (p<0.01), but the key comparison was the magnitude of the oil reduction rate.

[0127] From the test data in Table 4, it can be seen that all the shampoo treatment groups containing the composition of the application (Examples 1-6) can significantly inhibit the over-synthesis of SZ95 cells induced by linoleic acid, and the oil reduction rate is about 50%, indicating that it has a significant oil control effect. Although the comparative examples also show statistical differences, their oil reduction rates are much lower than those of the example groups, indicating that their oil control effect is weak.

[0128] The results of Nile red staining of cells in the application examples and comparative examples, and the fluorescence intensity are as follows:Figure 1 , 2 As shown, the in vitro lipid secretion results of SZ95 cells indicate that, as Figure 1 and 2 The results showed that after treatment with the application examples 1, 2, 4, and 5, the fluorescence intensity of cells in each example group was significantly reduced (P<0.01), the red fluorescence was weak and sparse, and the lipid droplets were reduced, indicating that the application examples 1, 2, 4, and 5 could inhibit the synthesis and secretion of lipids in SZ95 cells. In contrast, the cells in the comparative examples 1, 2, 4, and 5 showed strong and dense Nile Red staining fluorescence and a large accumulation of lipid droplets, indicating that the effect of inhibiting the synthesis and secretion of lipids in SZ95 cells was weak.

[0129] Examples 1 and 3 showed significantly better results than the corresponding conventional zinc (Comparative Example 1) and acid (Comparative Example 3) controls, demonstrating the advantages of bioactive zinc (Example 1) and the synergistic effect of gluconolactone and hydroxydecanoic acid (Example 3) in oil control in the composition of the present invention. The comparison between Examples 5 / 6 and Comparative Example 5 further demonstrates the importance of the synergistic effect of the active ingredients at effective concentrations. The combination of hydroxydecanoic acid (inhibiting lipase synthesis) and the two zinc raw materials (regulating sebaceous gland function) is one of the key mechanisms by which this composition achieves highly efficient oil control.

[0130] III. Human Efficacy Evaluation Experiment

[0131] We recruited 180 volunteers aged 18-40 (half male and half female), including those with recurrent dandruff (>6 months), a history of mild to moderate seborrheic dermatitis, and sensitive scalps. Exclusion criteria: pregnancy, scalp trauma, and use of medicated anti-dandruff products within the past 3 months. We used a half-scalp test model and a comparative model. After one month of use, participants evaluated their experience with the product. Evaluation dimensions included whether the product was effective in reducing dandruff, whether it was gentle and non-irritating, and a rating scale of 0-10, with higher scores indicating greater satisfaction. The percentage of participants who agreed with the product was calculated.

[0132] One month after the half-scalp test application examples and comparison examples, the scalp's moisture content and oil content were tested using a skin moisture testing probe called Moisture with pin probe. The probe, a pin-type design, directly measures the moisture content of the stratum corneum of the scalp. The testing principle is based on conductivity measurement of the skin's stratum corneum moisture content; a higher measurement value indicates higher scalp moisture content. The SM815 instrument directly measures sebum secretion on the scalp. The measurement time is 30 seconds. The light transmittance represents the sebum content on the skin surface of the measurement area. The measurement result is calculated by a microprocessor in units of 0 to 350. The smaller the measurement value, the lower the sebum content of the skin.

[0133] The VisioScan VC20plus-Corneofix instrument is used to take images of the skin surface through a uniform annular UV light (UVA) illuminating light source and a black and white high-resolution CCD camera, and the images are transmitted to the host computer for digital processing and analysis, and the image analysis software is used to quantify the dandruff coverage.

[0134] The test data is shown in Table 5.

[0135] Table 5 Test data

[0136]

[0137] As can be seen from the test data in Table 5, the stratum corneum moisture content of the application examples 1-6 is increased by >25%, which is significantly higher than that of the application comparative examples 1-5. Among them, the application examples 2 and 6 have better performance in increasing the moisture content of the stratum corneum, because the succinogluchan (molecular weight 2.0-3.0 x 10 6 Da) forms a three-dimensional hydrated film on the scalp, reduces transdermal water loss, synergizes with each component, enhances scalp moisturizing, and even better than the moisturizing effect of conventional sodium hyaluronate and ceramide.

[0138] The oil content reduction rate of the application examples is negative, and the absolute value is about 50%, which indicates that the composition added in the shampoo formula of the application examples 1-6 can achieve the effect of oil control by regulating sebum secretion and increasing the water content of the scalp.

[0139] The gluconolactone and double zinc system of the application example 3 jointly regulate the activity of sebaceous glands, reduce oil secretion from the source, and the effect is better than that of the acid oil control raw material of the application comparative example 3. The recognition rate of mildness dimension is as high as 100%, and other application examples 1-6 also perform excellently in scalp nourishment, dandruff reduction rate, and mildness and non-irritation dimensions, which indicates that the composition of the application is mild and non-burden on the scalp, and has a significant effect on regulating the scalp barrier and reducing dandruff.

[0140] As shown in Figure 3 , 4 , 5, the hair of the people before using the application example has a high reflective oily and greasy feeling, and the hair is sticky; after using the application example for 30 days, the oily and greasy feeling of the hair is significantly reduced, and the hair root is clean and fluffy; which indicates that the sebum secretion of the scalp is regulated by using the application example. The quantitative reduction of the scalp oil (>30%) is essentially a biomarker of the restoration of the homeostasis of the scalp barrier system, and the composition of the application can promote the restoration of the scalp environment to homeostasis by regulating the secretion of the scalp oil.

[0141] As shown in Figure 6 , 7As shown in FIGS. 8, the scalp of the human being has a large amount of silver-white dandruff attached before using the example, and the dandruff coverage and the size of the dandruff particles are obviously reduced after using the example for 30 days, the scalp is clean without dandruff, and the skin state of the scalp is smooth; the reduction or disappearance of the dandruff is a standard for realizing the fundamental regulation of the three dimensions of the microbial colonization, the keratin metabolism and the neuro-immune of the scalp barrier, and the continuous improvement indicates that the barrier function enters a stable state; it is shown that the composition of the present application can inhibit the harmful bacteria on the scalp, reduce the dandruff, and then promote the scalp to restore the normal barrier function in the dimensions of the microbial flora, the keratin metabolism and the immune barrier.

[0142] In summary, the multi-morphology zinc and organic acid composition for targeting the repair of the scalp barrier has the effects of regulating and inhibiting the secretion of oil, inhibiting Malassezia, enhancing the moisturizing capacity of the scalp, nourishing the scalp and being mild and non-irritating.

[0143] The above is only a preferred embodiment of the present application, and does not limit the present application in any form, so any simple modification, equivalent change and modification of the above embodiment according to the technical essence of the present application, which does not deviate from the technical solution content of the present application, still belongs to the scope of the technical solution of the present application.

Claims

1. A multi-form zinc and organic acid composition targeting scalp barrier repair, characterized in that: The composition comprises the following components by weight percentage: Yeast / zinc fermentation product 1-80%, polyaspartic acid chelated zinc 1-20%, gluconolactone 0.5-20%, hydroxydecanoic acid 0.5-6%, succinosaccharide 1-10%, balance water or other pharmaceutically / cosmetically acceptable carriers; The mass ratio of yeast / zinc fermentation product to polyaspartic acid chelated zinc was (1:1)-(8:1); the mass ratio of hydroxydecanoic acid to gluconolactone was (1:0.5)-(1:3).

2. The multimorphic zinc and organic acid composition for targeted scalp barrier repair as described in claim 1, characterized in that: The composition comprises the following components by weight percentage: Yeast / zinc fermentation product 20-80%, polyaspartic acid chelated zinc 1-20%, gluconolactone 1-10%, hydroxydecanoic acid 1-5%, succinosaccharide 1-5%, balance water or other pharmaceutically / cosmetically acceptable carriers. The mass ratio of yeast / zinc fermentation product to polyaspartic acid chelated zinc was (2.5:1)-(5:1); the mass ratio of hydroxydecanoic acid to gluconolactone was (1:0.7)-(1:3).

3. The multimorphic zinc and organic acid composition for targeted scalp barrier repair as described in claim 1, characterized in that: The composition comprises the following components by weight percentage: Yeast / zinc fermentation product 20-60%, polyaspartic acid chelated zinc 5-15%, gluconolactone 1.5-6%, hydroxydecanoic acid 2-4%, succinopolysaccharide 2-4%, balance water or other pharmaceutically / cosmetically acceptable carriers. The mass ratio of yeast / zinc fermentation product to polyaspartic acid chelated zinc was (2.5:1)-(5:1); the mass ratio of hydroxydecanoic acid to gluconolactone was (1:0.75)-(1:3).

4. The multimorphic zinc and organic acid composition for targeted scalp barrier repair as described in claim 1, characterized in that: The yeast / zinc fermentation product was obtained by the following method: The extremely cold-tolerant Saccharomyces cerevisiae strain CGMCC No.15873 was subjected to cyclic stress-stimulated fermentation with zinc sulfate. Taking advantage of the bioaccumulation ability of this yeast strain for zinc, the fermentation products were extracted and purified by bio-enzymatic hydrolysis technology. The total zinc content in the obtained fermentation products was 20-100 mg / kg, preferably 60-80 mg / kg. The specific steps are as follows: Using molasses purified from natural sugarcane as the carbon source and zinc sulfate as the zinc source, after strict sterilization, the extremely cold-tolerant Saccharomyces cerevisiae strain CGMCC No.15873 was activated and inoculated with additional yeast strains. In the initial stage, a low zinc concentration of 50-100 mg / L ZnSO4 was maintained. In the middle stage, based on sensor feedback on yeast growth rate, intracellular zinc accumulation rate, and metabolic activity parameters, the zinc concentration of the fermentation broth was increased in a programmed small gradient, increasing by 20-50 mg / L ZnSO4 each time. When a significant decrease in growth rate or plateau in accumulation rate was detected, the increase in zinc concentration was paused or the concentration was temporarily decreased. Fermentation was carried out at 70-80℃ for 10-15 hours, followed by enzymatic hydrolysis with protease for 20-30 hours, and thermal treatment at 100-120℃ for 2-5 hours. Immediately after enzymatic hydrolysis, the mixture was centrifuged at low temperature and separated using an ultrafiltration membrane to rapidly separate the zinc-rich soluble components. The supernatant was collected to obtain the yeast / zinc fermentation product.

5. The multimorphic zinc and organic acid composition for targeted scalp barrier repair as described in claim 1, characterized in that: The total zinc content in the polyaspartic acid chelated zinc is 400-800 mg / kg, preferably 450-650 mg / kg; its polymer weight-average molecular weight (Mw) is 10000-50000 Da, preferably 20000-35000 Da.

6. The multimorphic zinc and organic acid composition for targeted scalp barrier repair as described in claim 1, characterized in that: The succinyl polysaccharide is a polysaccharide compound consisting of multiple glucose units linked by glycosidic bonds, with succinyl groups (-CO-CH2-CH2-COO-) attached to the glucose units. Its weight-average molecular weight is 1.5 × 10⁻⁶. 6 Da-3.5×10 6 Da, preferably 2.0 × 10 6 Da-3.0×10 6 Da.

7. The method for preparing the multimorphic zinc and organic acid composition targeting scalp barrier repair according to any one of claims 1-6, characterized in that, Includes the following steps: 1) Add the prescribed amount of water and succinosaccharide to the reaction vessel and perform high-speed homogenization dispersion at a speed of 2000-3000 rpm; 2) Heat to 80-85℃ and stir at 200-500 rpm for 20-30 minutes to ensure that the succinyl polysaccharide is completely dissolved and homogeneous; 3) Cool the solution obtained in step 2) to 40-45℃; 4) Add the formulated amounts of yeast / zinc fermentation product, polyaspartic acid chelated zinc, gluconolactone, and hydroxydecanoic acid sequentially to the cooled solution, and stir evenly at a stirring speed of 200-500 rpm. 5) Cool the mixture obtained in step 4) to 37-39℃; filter the mixture using a filter screen to obtain the multi-form zinc and organic acid composition for targeted scalp barrier repair.

8. The method for preparing the multimorphic zinc and organic acid composition targeting scalp barrier repair as described in claim 7, characterized in that: After step 4) or step 5), adjust the pH of the pH adjustment composition to 4.0-5.

5.

9. The application of the multimorphic zinc and organic acid composition for targeted scalp barrier repair as described in claim 7 in the preparation of scalp care products, characterized in that: The hair care product is selected from one or more of shampoo, hair lotion, scalp serum, scalp gel, and scalp spray; the composition is added to the hair care product at a low temperature; a more preferred addition temperature is 10-45°C, and the most preferred addition temperature is room temperature.

10. The application of the multimorphic zinc and organic acid composition for targeted scalp barrier repair as described in claim 9, characterized in that: The hair care product mentioned is shampoo; The shampoo comprises the following components by weight percentage: Phase A: Water balance, guar gum hydroxypropyltrimethylammonium chloride (low molecular weight) 0.2%, guar gum hydroxypropyltrimethylammonium chloride (high molecular weight) 0.1%, citric acid 0.05%; Phase B: 6% cocamidopropyl betaine, 15% sodium lauryl ether sulfate, 6% lauryl hydroxysulfonate betaine, 0.3% cocamidopropyl betaine, 0.8% ethylene glycol distearate, 0.2% cetearyl alcohol, and 0.2% hydrogenated castor oil; Phase C: Emulsified silicone oil 1785POE 1.5%, emulsified silicone oil 7137POE 1.2%, phenoxyethanol 0.4%, sodium benzoate 0.4%, glycerin 1.5%, fragrance 0.5%, sodium chloride 0.8%; Phase D: 4% of the multimorphic zinc and organic acid composition targeting scalp barrier repair; The preparation process of the shampoo Includes the following steps: At room temperature, while homogenizing, add phase A raw material to the emulsifying pot at a homogenizing speed of 2500 RPM / min for 5 minutes. Then, start stirring at 300 RPM / min and heat to 90°C with steam. Add phase B raw material and maintain the temperature for 30 minutes. Then, turn on the condenser to cool to 50-55°C and maintain the temperature while stirring for 30 minutes. Continue cooling to 40°C, add phase C and phase D raw materials, and stir for 20 minutes until homogeneous. Then, cool to 38°C. After passing inspection, filter and bottle the product.

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