Anti-dandruff composition and preparation method and application thereof
By using anti-dandruff compositions prepared by Chinese medicinal materials such as Sophora root, windproof root, Magnolia bark, licorice root and piercing lotus leaf, the safety and effectiveness of chemical fungicides in existing anti-dandruff products were solved, and effective inhibition was achieved Malassezia furf, improves hair environment and is safe and non-irritating.
Patent Information
- Application Number
- CN202311527239.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-11-16
- Publication Date
- 2025-02-07
- Estimated Expiration
- 2043-11-16
AI Technical Summary
The chemical fungicides used in existing anti-dandruff products have the risks of residual, irritating and carcinogenic sensitization, and the effect is not significant enough, making it difficult to meet the market's demand for pure natural, safe and non-irritating anti-dandruff compositions.
An anti-dandruff composition composed of Chinese medicinal materials such as Sophora root, windproof root, Magnolia bark, licorice root and piercing lotus leaves is prepared through ethanol extraction and distillation and other processes to prepare a green, safe and non-irritating anti-dandruff product.
This anti-dandruff composition can effectively inhibit the reproduction and production of Malase furfus, reduce the production of dandruff, improve the hair microbial environment, restore the hair to blackness and smoothness, and also has the effect of antioxidant and regulating sebum secretion, which is safe and non-irritating , suitable for long-term use.
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Abstract
Description
Technical Field
[0001] The present application relates to the technical field of daily chemicals, and in particular to an anti-dandruff composition and a preparation method and application thereof. Background Art
[0002] Dandruff is a common problem that bothers people's lives. There are many reasons for dandruff, such as irregular diet, reduced gastrointestinal function of decomposing oil, resulting in excessive scalp oil secretion, and residual oil that cannot be washed away when washing; excessive shampooing, which causes the scalp to produce a stress response and secrete more oil or improper use of maintenance cleaning products, causing a large amount of polymers to polymerize on the hair to form a protective film; microbial imbalance; scalp cell dysfunction; seasonal skin diseases, etc. The most common causes are microbial imbalance and scalp cell dysfunction. Therefore, a dandruff composition product that inhibits microbial reproduction and controls oil secretion is needed to meet market demand.
[0003] CN116869900A discloses that the anti-dandruff shampoo comprises the following components: surfactant, anti-dandruff composition, moisturizing lubricant, thickener, active extract, preservative, chelating agent, other auxiliary agents and pure water. The dichlorobenzyl alcohol and climbazole in the anti-dandruff composition act synergistically to significantly enhance the antibacterial effect of the shampoo, and the active extract is combined to further enhance the antibacterial effect of the shampoo, so that the shampoo can not only inhibit bacterial growth and clean scalp oil, thereby achieving the effect of inhibiting dandruff generation, but also soothe the scalp and nourish the hair roots.
[0004] However, the ingredients of anti-dandruff products currently on the market are all subject to regulatory restrictions and quantity control. For example, zinc pyrithione, triclosan, climbazole, piroctone olamine salt, etc. are all chemical fungicides that can effectively kill microorganisms, but have residual and irritating properties. In addition, their use is highly controversial in the European Union and the Americas, and there are risks of carcinogenicity and allergenicity. Therefore, it is necessary to develop a natural, safe, non-irritating, and effective anti-dandruff composition. Summary of the invention
[0005] The present application provides an anti-dandruff composition and a preparation method and application thereof. By cooperating with each other, the components can effectively inhibit the production of Malassezia furfur, inhibit oil secretion, scavenge the free radical DPPH, improve the scalp barrier function, reduce problems such as scalp itching, dryness and dandruff, and realize a green, safe and non-irritating anti-dandruff composition.
[0006] In order to solve the above technical problems, in the first aspect, the present application provides an anti-dandruff composition, comprising the following components in weight percentage:
[0007] Sophora flavescens root 1%-5%, Saposhnikovia root 0.5%-5%, Magnolia officinalis bark 0.5%-2%, Licorice root 0.3%-2%, Andrographis paniculata leaf 0.1%-1%, and the rest are solvents.
[0008] In one embodiment, the anti-dandruff composition comprises the following components in weight percentage:
[0009] Sophora flavescens root 1%, Saposhnikovia root 5%, Magnolia officinalis bark 2%, Licorice root 1.8%, Andrographis paniculata leaf 0.2%, and the rest are solvents.
[0010] In one embodiment, the solvent is composed of components in the following mass ratio: the mass ratio of polyol to deionized water is 1:2 to 10; the polyol includes one or more of butanediol, isoprene glycol, 1,2-ethylene glycol, 1,2-pentanediol and 1,3-propylene glycol.
[0011] In one embodiment, the anti-dandruff composition further comprises 0.5% to 2% of preservatives.
[0012] In one embodiment, the preservative is one or more of caprylhydroxamic acid, phenoxyethanol, methylparaben, chlorphenesin, p-hydroxyacetophenone, sodium benzoate, potassium sorbate and ethylhexylglycerin.
[0013] Optionally, the extraction part of the Sophora flavescens root is the root, produced in Huanggang, Hubei; the extraction part of the Saposhnikovia root is the root, produced in Taikang, Heilongjiang; the extraction part of the Magnolia officinalis bark is the bark, produced in Dujiangyan, Sichuan; the extraction part of the Licorice root is the sub-root, produced in Wuwei, Gansu; and the extraction part of the Andrographis paniculata leaf is the leaf, produced in Maoming, Guangdong.
[0014] The root of Sophora flavescens contains matrine and cytisine, which can be used as medicine to clear away heat and dampness, have antibacterial and anti-inflammatory effects, and strengthen the stomach and expel parasites. It is often used to treat symptoms such as skin itching, neurasthenia, indigestion, and constipation.
[0015] The root of Saposhnikovia root contains cimicifuga, coumarins and Saposhnikovia polysaccharide, which has the effects of dispelling wind and dampness, soothing the liver and detoxifying. It is often used to treat symptoms such as rheumatism, dysentery, infantile malnutrition, rash and prolapse of the anus.
[0016] Magnolia officinalis bark contains magnolia officinalis, tetrahydromagnolia officinalis, isomagnolia officinalis and magnolia officinalis; it has the effects of removing dampness and relieving stagnation, promoting qi and relieving asthma, digesting food and eliminating phlegm, expelling wind and relieving pain; it can be used to treat symptoms such as dampness blocking the middle part of the body, abdominal distension, food stagnation and qi stagnation, abdominal distension and constipation, phlegm and cough.
[0017] Licorice root contains glycyrrhizin, licorice and isoflavones. It has the effects of tonifying the spleen and replenishing qi, clearing away heat and detoxifying, removing phlegm and relieving cough, relieving pain and harmonizing various medicines. It can be used for symptoms such as spleen and stomach weakness, fatigue, palpitations and shortness of breath, cough with sputum, abdominal pain, cramps and pain in the limbs, and carbuncles and sores.
[0018] Andrographolide, andrographolide, andrographolide C, homoandrographolide, penynolide, andrographolane, andrographolone and andrographolide, etc., can be used as medicine to clear away heat and detoxify, reduce inflammation, reduce swelling and relieve pain. It is often used for colds and fever, sore throat, mouth sores, sudden cough, diarrhea, dysentery, hot and painful stranguria, carbuncles, ulcers, snake and insect bites.
[0019] The anti-dandruff composition can play a synergistic role by compounding the root of Sophora flavescens, the root of Saposhnikovia divaricata, the bark of Magnolia officinalis, the root of Licorice and the leaf of Andrographis paniculata. Through the synergistic effect, the reproduction and generation of Malassezia furfur can be effectively inhibited, thereby reducing the generation of dandruff, improving the microbial environment of hair, and restoring the hair to black, shiny and smooth. Through the synergistic effect, the activity of 5-α reductase can be inhibited, sebum secretion can be regulated, sebum secretion can be balanced, hair follicle blockage can be reduced, hair loss and microbial reproduction can be improved, and the problems of dry itching caused by greasy hair and airtightness can be improved. Through the synergistic effect, the generation of DPPH free radicals can be effectively removed, the oxidation of unsaturated fatty acids, triglycerides, cholesterol, etc. can be slowed down, the oxidation and taste change of secreted oil can be improved, and the inflammation caused by the blockage of scalp oil secretion can be relieved and reduced. At the same time, the anti-dandruff composition adopts Chinese medicine ingredients, is safe and non-irritating, can be used for a long time, does not leave residue, and has obvious effect in improving dandruff.
[0020] In a second aspect, the present application provides a method for preparing an anti-dandruff composition, comprising the following steps:
[0021] Step 1: Weigh the roots of Sophora flavescens, Saposhnikovia divaricata, Magnolia officinalis bark, Licorice root and Andrographis paniculata leaf respectively, crush them into 80-250 mm using a crusher and mix them for later use;
[0022] Step 2: Weigh the mixture of step 1 and 50% ethanol in a mass ratio of 1:10-50, reflux extract in a constant temperature water bath at 80°C-90°C for 120min-150min, cool naturally to room temperature, and filter to obtain extract I for later use;
[0023] Step 3: The filter residue of step 2 is mixed with 60% ethanol in a mass ratio of 1:10-50, and reflux extraction is performed in a constant temperature water bath at 80°C-90°C for 120min-150min, and then naturally cooled to room temperature, and filtered to obtain extract II for standby use;
[0024] Step 4: The filter residue of step 3 is mixed with 70% ethanol in a mass ratio of 1:10-50, and reflux extraction is performed in a constant temperature water bath at 80°C-90°C for 120min-150min, and then naturally cooled to room temperature, and filtered to obtain extract III for standby use;
[0025] Step 5: Combine the extracts I, II and III, let stand for 12 hours, take the supernatant and add it to a rotary bottle, put it in a rotary evaporator at 85°C to 95°C in a water bath for compression distillation for 120min to 150min, recover ethanol, and cool it naturally to room temperature to obtain concentrated solution IV;
[0026] Step 6: Add 95% ethanol at a mass ratio of 1:50-70 to the concentrated solution IV in step 5 under stirring with a stirrer, stir for 30 minutes, let stand for 12 hours, take the supernatant after precipitation is complete, add it to a rotary bottle, put it in a rotary evaporator in a water bath at 85°C-95°C for compression distillation for 120min-150min, recover ethanol, and cool it naturally to room temperature to obtain a concentrated solution V;
[0027] Step 7: Put the concentrated liquid V in step 6 into a beaker, add solvent, heat to 75°C ~ 85°C, weigh the preservative, dissolve it in the container and evenly add it to the beaker, stir at 35r / min ~ 45r / min for 30min ~ 40min, cool to room temperature, put it into a plastic container, put it in a refrigerator at 0°C ~ 5°C and let it stand for 12h. After precipitation is complete, filter with a -0.05MPa ~ -0.1MPa pressure vacuum pump and 800 mesh filter cloth to obtain a clear liquid, i.e., the anti-dandruff composition.
[0028] In one embodiment, the preparation method of the anti-dandruff composition comprises the following steps:
[0029] Step 1: Weigh the roots of Sophora flavescens, Saposhnikovia divaricata, Magnolia officinalis bark, Licorice root and Andrographis paniculata leaf respectively, crush them into 200 mm using a crusher and mix them for later use;
[0030] Step 2: Weigh the mixture of step 1 and 50% ethanol in a mass ratio of 1:10, reflux extract in a constant temperature water bath at 90°C for 120 minutes, cool naturally to room temperature, and filter to obtain extract I for later use;
[0031] Step 3: The filter residue of step 2 was mixed with 60% ethanol in a mass ratio of 1:50, and refluxed in a constant temperature water bath at 88°C for 130 minutes, then naturally cooled to room temperature, and filtered to obtain extract II for later use;
[0032] Step 4: The filter residue of step 3 was mixed with 70% ethanol in a mass ratio of 1:30, and refluxed in a constant temperature water bath at 82°C for 150 minutes, then naturally cooled to room temperature, and filtered to obtain extract III for later use;
[0033] Step 5: Combine the extracts I, II and III, let stand for 12 hours, take the supernatant and add it to a rotary bottle, put it in a water bath 85°C rotary evaporator for compression distillation for 150 minutes, recover ethanol, and naturally cool to room temperature to obtain concentrated solution IV;
[0034] Step 6: Add 95% ethanol at a mass ratio of 1:60 to the concentrated solution IV in step 5 under stirring with a stirrer, stir for 30 minutes, let stand for 12 hours, take the supernatant after precipitation is complete, add it to a rotary bottle, put it in a water bath at 95°C rotary evaporator for compression distillation for 120 minutes, recover ethanol, and naturally cool to room temperature to obtain a concentrated solution V;
[0035] Step 7: Put the concentrated liquid V in step 6 into a beaker, add solvent, heat to 85°C, weigh the preservative, dissolve it in the container and add it to the beaker, stir at 35r / min for 40min, cool to room temperature, put it into a plastic container, put it in a refrigerator at 2°C and let it stand for 12h. After precipitation is complete, filter with a -0.09MPa pressure vacuum pump and 800 mesh filter cloth to obtain a clear liquid, i.e., the anti-dandruff composition.
[0036] In a third aspect, the present application provides an application of an anti-dandruff composition in the preparation of an anti-dandruff product, wherein the anti-dandruff composition is added in an amount of 1% to 10% in the anti-dandruff product.
[0037] In one embodiment, the anti-dandruff composition is added in an amount of 3% to 10% in the anti-dandruff product.
[0038] In one embodiment, the anti-dandruff product includes shampoo, hair mask, anti-dandruff water, conditioner or hair growth liquid.
[0039] The preparation method of the anti-dandruff composition is simple, low in cost, and conducive to industrial production. The product is convenient to use, safe and non-irritating, can be used for a long time, and has obvious effect in improving dandruff. DETAILED DESCRIPTION
[0040] In order to make the above-mentioned purpose, features and advantages of the present invention more obvious and easy to understand, the specific embodiments of the present invention are described in detail below. In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without violating the connotation of the present invention, so the present invention is not limited by the specific embodiments disclosed below.
[0041] As used herein, the term "prepared from" is synonymous with "comprising." As used herein, the terms "comprising," "including," "having," "containing," or any other variation thereof, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises the listed elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
[0042] When amount, concentration or other value or parameter is expressed as range, preferred range or a series of upper preferred value and lower preferred value limit range, this should be understood as specifically disclosing all ranges formed by any pairing of any range upper limit or preferred value and any range lower limit or preferred value, regardless of whether the range is disclosed separately. For example, when disclosing range "1 to 5", described range should be interpreted as including range "1 to 4", "1 to 3", "1 to 2", "1 to 2 and 4 to 5", "1 to 3 and 5" etc. When numerical range is described in this article, unless otherwise stated, the range is intended to include its end value and all integers and fractions within the range.
[0043] In addition, the indefinite articles "a" and "an" before the elements or components of the present invention have no restrictions on the quantity requirements (i.e. the number of occurrences) of the elements or components. Therefore, "a" or "an" should be interpreted as including one or at least one, and the elements or components in the singular form also include the plural form, unless the number is obviously intended to be in the singular form.
[0044] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used herein in the specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The term "and / or" used herein includes any and all combinations of one or more related listed items.
[0045] Embodiment 1:
[0046] Step 1: Weigh 3% of Sophora flavescens root, 4.2% of Saposhnikovia root, 1% of Magnolia officinalis bark, 1% of Licorice root and 0.8% of Andrographis paniculata leaf respectively by weight percentage, crush them into 250mm with a crusher and mix them for later use;
[0047] Step 2: Weigh the mixture of step 1 and 50% ethanol in a mass ratio of 1:10, reflux extract in a constant temperature water bath at 85°C for 135 minutes, cool naturally to room temperature, and filter to obtain extract I for later use;
[0048] Step 3: The filter residue of step 2 was mixed with 60% ethanol in a mass ratio of 1:40, and refluxed in a constant temperature water bath at 88°C for 130 minutes, then naturally cooled to room temperature, and filtered to obtain extract II for later use;
[0049] Step 4: The filter residue of step 3 was mixed with 70% ethanol in a mass ratio of 1:40, and refluxed in a constant temperature water bath at 82°C for 130 minutes, then naturally cooled to room temperature, and filtered to obtain extract III for later use;
[0050] Step 5: Combine the extracts I, II and III, let stand for 12 hours, take the supernatant and add it to a rotary bottle, put it in a water bath 85°C rotary evaporator for compression distillation for 145 minutes, recover ethanol, and cool it naturally to room temperature to obtain concentrated solution IV;
[0051] Step 6: Add 95% ethanol at a mass ratio of 1:55 to the concentrated solution IV in step 5 under stirring with a stirrer, stir for 30 minutes, let stand for 12 hours, take the supernatant after precipitation is complete, add it to a rotary bottle, put it in a rotary evaporator at 90°C in a water bath for compression distillation for 140 minutes, recover ethanol, and cool it naturally to room temperature to obtain a concentrated solution V;
[0052] Step 7: Put the concentrated solution V in step 6 into a beaker, add 11% butanediol and deionized water to 100%, heat to 85°C, weigh 0.54% phenoxyethanol, dissolve it in a container and evenly add it to the beaker, stir at 40 r / min for 35 minutes, cool to room temperature, put it into a plastic container, put it in a refrigerator at 3°C and let it stand for 12 hours. After precipitation is complete, filter with a -0.08 MPa pressure vacuum pump and 800 mesh filter cloth to obtain a clear liquid, i.e., the anti-dandruff composition.
[0053] Example 2
[0054] Step 1: Weigh 5% of Sophora flavescens root, 1% of Saposhnikovia root, 2% of Magnolia officinalis bark, 1.3% of Licorice root and 0.7% of Andrographis paniculata leaf respectively by weight percentage, crush them into 100 mm with a crusher and mix them for later use;
[0055] Step 2: Weigh the mixture of step 1 and 50% ethanol in a mass ratio of 1:30, reflux extract in a 90°C constant temperature water bath for 120 min, cool naturally to room temperature, and filter to obtain extract I for later use;
[0056] Step 3: The filter residue of step 2 was mixed with 60% ethanol in a mass ratio of 1:30, and refluxed in a constant temperature water bath at 90°C for 120 minutes, then naturally cooled to room temperature, and filtered to obtain extract II for later use;
[0057] Step 4: The filter residue of step 3 was mixed with 70% ethanol in a mass ratio of 1:30, and refluxed in a constant temperature water bath at 90°C for 120 minutes, then naturally cooled to room temperature, and filtered to obtain extract III for later use;
[0058] Step 5: Combine the extracts I, II and III, let stand for 12 hours, take the supernatant and add it to a rotary bottle, put it in a water bath 85°C rotary evaporator for compression distillation for 125 minutes, recover ethanol, and cool it naturally to room temperature to obtain concentrated solution IV;
[0059] Step 6: Add 95% ethanol at a mass ratio of 1:70 to the concentrated solution IV in step 5 under stirring with a stirrer, stir for 30 minutes, let stand for 12 hours, take the supernatant after precipitation is complete, add it to a rotary bottle, put it in a water bath at 95°C rotary evaporator for compression distillation for 120 minutes, recover ethanol, and naturally cool to room temperature to obtain a concentrated solution V;
[0060] Step 7: Put the concentrated solution V in step 6 into a beaker, add 10% isopentyl glycol, 0.5% 1,2-hexanediol, and deionized water to 100%, heat to 85°C, weigh 0.5% p-hydroxyacetophenone, dissolve it in a container and evenly add it to the beaker, stir at 45 r / min for 30 minutes, cool to room temperature, put it into a plastic container, put it in a refrigerator at 0°C and let it stand for 12 hours. After precipitation is complete, filter with a -0.1 MPa pressure vacuum pump and 800 mesh filter cloth to obtain a clear liquid, i.e., the anti-dandruff composition.
[0061] Example 3
[0062] Step 1: Weigh 1% of Sophora flavescens root, 0.5% of Saposhnikovia root, 2% of Magnolia officinalis bark, 1.8% of Licorice root and 0.2% of Andrographis paniculata leaf respectively by weight percentage, crush them into 200mm with a crusher and mix them for later use;
[0063] Step 2: Weigh the mixture of step 1 and 50% ethanol in a mass ratio of 1:10, reflux extract in a constant temperature water bath at 90°C for 120 minutes, cool naturally to room temperature, and filter to obtain extract I for later use;
[0064] Step 3: The filter residue of step 2 was mixed with 60% ethanol in a mass ratio of 1:50, and refluxed in a constant temperature water bath at 88°C for 130 minutes, then naturally cooled to room temperature, and filtered to obtain extract II for later use;
[0065] Step 4: The filter residue of step 3 was mixed with 70% ethanol in a mass ratio of 1:30, and refluxed in a constant temperature water bath at 82°C for 150 minutes, then naturally cooled to room temperature, and filtered to obtain extract III for later use;
[0066] Step 5: Combine the extracts I, II and III, let stand for 12 hours, take the supernatant and add it to a rotary bottle, put it in a water bath 85°C rotary evaporator for compression distillation for 150 minutes, recover ethanol, and naturally cool to room temperature to obtain concentrated solution IV;
[0067] Step 6: Add 95% ethanol at a mass ratio of 1:60 to the concentrated solution IV in step 5 under stirring with a stirrer, stir for 30 minutes, let stand for 12 hours, take the supernatant after precipitation is complete, add it to a rotary bottle, put it in a water bath at 95°C rotary evaporator for compression distillation for 120 minutes, recover ethanol, and naturally cool to room temperature to obtain a concentrated solution V;
[0068] Step 7: Put the concentrated solution V in step 6 into a beaker, add 2% 1,2-pentanediol, 21% 1,3-propylene glycol, and deionized water to 100%, heat to 85°C, weigh 0.1% chlorphenesin and 0.5% ethylhexylglycerol, dissolve them evenly in a container and add them to the beaker, stir at 35 r / min for 40 minutes, cool to room temperature, put into a plastic container, put it in a refrigerator at 2°C and let it stand for 12 hours. After precipitation is complete, filter with a -0.09 MPa pressure vacuum pump and 800 mesh filter cloth to obtain a clear liquid, i.e., the anti-dandruff composition.
[0069] Example 4
[0070] Step 1: Weigh 3% of Sophora flavescens root, 3.5% of Saposhnikovia root, 0.5% of Magnolia officinalis bark, 2% of Licorice root and 1% of Andrographis paniculata leaf respectively by weight, crush them into 120 mm with a crusher and mix them for later use;
[0071] Step 2: Weigh the mixture of step 1 and 50% ethanol in a mass ratio of 1:10, reflux extract in a constant temperature water bath at 90°C for 120 minutes, cool naturally to room temperature, and filter to obtain extract I for later use;
[0072] Step 3: The filter residue of step 2 was mixed with 60% ethanol in a mass ratio of 1:50, and refluxed in a constant temperature water bath at 85°C for 120 minutes, then naturally cooled to room temperature, and filtered to obtain extract II for later use;
[0073] Step 4: The filter residue of step 3 was mixed with 70% ethanol in a mass ratio of 1:50, and refluxed in a constant temperature water bath at 80°C for 120 minutes, then naturally cooled to room temperature, and filtered to obtain extract III for later use;
[0074] Step 5: Combine the extracts I, II and III, let stand for 12 hours, take the supernatant and add it to a rotary bottle, put it in a water bath 85°C rotary evaporator for compression distillation for 150 minutes, recover ethanol, and naturally cool to room temperature to obtain concentrated solution IV;
[0075] Step 6: Add 95% ethanol at a mass ratio of 1:50 to the concentrated solution IV in step 5 under stirring with a stirrer, stir for 30 minutes, let stand for 12 hours, take the supernatant after precipitation is complete, add it to a rotary bottle, put it in a rotary evaporator in a water bath at 85°C for compression and distillation for 135 minutes, recover ethanol, and cool it naturally to room temperature to obtain a concentrated solution V;
[0076] Step 7: Put the concentrated solution V in step 6 into a beaker, add 21% butanediol and deionized water to 100%, heat to 85°C, weigh 0.5% sodium benzoate and 0.5% potassium sorbate and add them into the beaker, stir at 42 r / min for 30 min, cool to room temperature, put into a plastic container, put it in a refrigerator at 1°C and let it stand for 12 h. After precipitation is complete, filter with a -0.05 MPa pressure vacuum pump and 800 mesh filter cloth to obtain a clear liquid, i.e., the anti-dandruff composition.
[0077] Example 5
[0078] Step 1: Weigh 4.2% of Sophora flavescens root, 2.5% of Saposhnikovia root, 2% of Magnolia officinalis bark, 0.3% of Licorice root and 1% of Andrographis paniculata leaf respectively by weight percentage, crush them into 80 mm with a crusher and mix them for later use;
[0079] Step 2: Weigh the mixture of step 1 and 50% ethanol in a mass ratio of 1:35, reflux extract in a constant temperature water bath at 80°C for 150 minutes, cool naturally to room temperature, and filter to obtain extract I for later use;
[0080] Step 3: The filter residue of step 2 was mixed with 60% ethanol in a mass ratio of 1:20, and refluxed in a constant temperature water bath at 85°C for 125 minutes, then naturally cooled to room temperature, and filtered to obtain extract II for later use;
[0081] Step 4: The filter residue of step 3 was mixed with 70% ethanol in a mass ratio of 1:20, and refluxed in a constant temperature water bath at 90°C for 120 minutes, then naturally cooled to room temperature, and filtered to obtain extract III for later use;
[0082] Step 5: Combine the extracts I, II and III, let stand for 12 hours, take the supernatant and add it to a rotary bottle, put it in a water bath 85°C rotary evaporator for compression distillation for 125 minutes, recover ethanol, and cool it naturally to room temperature to obtain concentrated solution IV;
[0083] Step 6: Add 95% ethanol at a mass ratio of 1:50 to the concentrated solution IV in step 5 under stirring with a stirrer, stir for 30 minutes, let stand for 12 hours, take the supernatant after precipitation is complete, add it to a rotary bottle, put it in a rotary evaporator in a water bath at 95°C for compression distillation for 150 minutes, recover ethanol, and cool it naturally to room temperature to obtain a concentrated solution V;
[0084] Step 7: Put the concentrated solution V in step 6 into a beaker, add 11% butanediol, 0.16% 1,2-hexanediol, and deionized water to 100%, heat to 85°C, weigh 0.16% phenoxyethanol and 0.08% chlorphenesin, add to the beaker, stir at 38 r / min for 30 minutes, cool to room temperature, put into a plastic container, put it in a refrigerator at 5°C and let it stand for 12 hours. After precipitation is complete, filter with a -0.1 MPa pressure vacuum pump and 800 mesh filter cloth to obtain a clear liquid, i.e., the anti-dandruff composition.
[0085] Comparative Example 1
[0086] Compared with Example 1, the root of Sophora flavescens was replaced by deionized water, and the contents of other components and the process remained unchanged.
[0087] Comparative Example 2
[0088] Compared with Example 1, the root of Sophora flavescens is replaced by the root of Saposhnikovia divaricata, and the contents of other components and the process remain unchanged.
[0089] Comparative Example 3
[0090] Compared with Example 1, the root of Sophora flavescens and the bark of Magnolia officinalis are replaced by the root of Saposhnikovia divaricata and the root of Licorice, and the contents of other components and the process remain unchanged.
[0091] Comparative Example 4
[0092] Compared with Example 2, the Magnolia officinalis bark is replaced by Andrographis paniculata leaf, and the contents of other components and the process remain unchanged.
[0093] Comparative Example 5
[0094] Compared with Example 2, the Andrographis paniculata leaf was replaced by deionized water, and the contents of other components and the process remained unchanged.
[0095] Table 1 Content of each component of Examples 1-5 and Comparative Examples 1-5 (unit: weight percentage)
[0096]
[0097]
[0098] The technical standards for anti-dandruff composition products are as follows:
[0099] Appearance: Colorless to light brown transparent liquid;
[0100] pH:5.0-7.0
[0101] Stability (cold resistance): kept in a (-8±2)℃ refrigerator for 24 hours, no stratification after returning to room temperature;
[0102] Stability (heat resistance): Keep in a (40±1)℃ constant temperature box for 24 hours, and there is no stratification after returning to room temperature;
[0103] Total colony count: <10CFU / g;
[0104] Mold and yeast: <10CFU / g;
[0105] Thermotolerant coliform bacteria: shall not be detected;
[0106] Staphylococcus aureus: shall not be detected;
[0107] Pseudomonas aeruginosa: shall not be detected;
[0108] Heavy metals (lead ≤ 10 mg / kg, mercury ≤ 1 mg / kg, arsenic ≤ 2 mg / kg, cadmium ≤ 5 mg / kg).
[0109] The anti-dandruff compositions of Examples 1-5 and Comparative Examples 1-5 are added to anti-dandruff products. For example, 3% by weight is added to shampoo. The formula of the anti-dandruff shampoo is shown in Table 2:
[0110] Table 2 Anti-dandruff shampoo formula
[0111]
[0112]
[0113] The anti-dandruff shampoos of Examples 1-5 and Comparative Examples 1-5 were tested respectively, and the specific testing methods and test results are as follows:
[0114] 1. In vitro test - Malassezia furfur inhibition rate test:
[0115] Referring to 7.3 Test method for antibacterial effect of antibacterial daily chemical products (suspension quantitative method) in QB / T 2738-2012 Evaluation method for antibacterial and antibacterial effects of daily chemical products, the test data results are shown in Table 3.
[0116] Test reagents and equipment: olive oil agar medium, biochemical incubator, biological safety cabinet, low-temperature constant temperature bath, electronic balance.
[0117] Test bacteria: Malassezia furfur (ATCC 44344); action concentration: 1:1; action time: 2 min.
[0118] Table 3 Malassezia furfur inhibition rate
[0119] Test samples Antibacterial rate (%) Example 1 90.99 Example 2 92.97 Example 3 92.98 Example 4 92.31 Example 5 92.31 Comparative Example 1 22.55 Comparative Example 2 29.33 Comparative Example 3 6.95 Comparative Example 4 13.69 Comparative Example 5 21.45
[0120] According to the results in Table 3, the antibacterial rates of Examples 1-5 on Malassezia furfur are all greater than 90%, indicating that the products have a strong antibacterial effect; while the antibacterial rates of Comparative Examples 1-5 on Malassezia furfur are all less than 50%, indicating that the products obviously do not meet the minimum antibacterial requirements; in summary, the anti-dandruff composition of the present invention has a strong antibacterial effect on Malassezia furfur, can effectively inhibit the secondary growth of Malassezia furfur on the scalp, causing dandruff, and can help consumers improve the trouble of dandruff.
[0121] 2. In vitro test - free radical scavenging antioxidant test:
[0122] (1) Reagent preparation
[0123] Ethanol solution of 1,1-diphenyl-2-trinitrophenylhydrazine (DPPH): weigh 25 mg DPPH, dissolve it in anhydrous ethanol and make up to volume in a 1000 mL volumetric flask. The DPPH concentration is 25 mg / L. Store in a low temperature refrigerator away from light. The validity period is 7 days.
[0124] (2) Test method
[0125] S1: Add 0.1 mL of 20 mg / L DPPH test solution and 0.1 mL of test sample to the test tube, add anhydrous ethanol to the total volume to 3 mL, shake well, react in the dark for 30 minutes, take 1.0 mL and transfer to a 96-well plate to measure the absorbance at a wavelength of 517 nm;
[0126] S2: Add 2.9 mL of anhydrous ethanol and 0.1 mL of the test sample to the test tube, shake well, and react for 30 minutes in the dark. Then, take 1.0 mL and transfer it to a 96-well plate to measure the absorbance at a wavelength of 517 nm.
[0127] S3: Add 0.1 mL of 20 mg / L DPPH test solution and 2.9 mL of anhydrous ethanol to the test tube, shake well, react for 30 minutes in the dark, take 1 mL and transfer to a 96-well plate to measure the absorbance at a wavelength of 517 nm.
[0128] DPPH is a stable, long-lived free radical. Its ethanol solution is dark purple and has strong absorption near 517nm. When a free radical scavenger is present, the light absorption of the DPPH ethanol solution is weakened due to its single electron pairing. The degree of fading of the DPPH ethanol solution is linearly related to the number of electrons it accepts. This can be used to evaluate the ability of the test sample to scavenge free radicals. That is, the greater the scavenging rate, the stronger its free radical scavenging antioxidant ability.
[0129] The calculation formula of sample DPPH free radical scavenging rate is:
[0130]
[0131] A1 is the absorbance value of the system after DPPH is removed from the sample to be tested; A2 is the absorbance value of the system after DPPH is removed from the sample blank control; A3 is the absorbance value of the reaction system before adding the drug.
[0132] Table 4 DPPH free radical scavenging rate test data results
[0133] Sample name Clearance rate (%) Example 1 55±1.25 Example 2 56±1.65 Example 3 58±1.25 Example 4 56±1.15 Example 5 56±1.24 Comparative Example 1 21±0.25 Comparative Example 2 18±0.25 Comparative Example 3 17±0.35 Comparative Example 4 12±1.05 Comparative Example 5 14±0.25
[0134] From the test results in Table 4, it can be seen that Examples 1-5 have obvious ability to scavenge DPPH free radicals, with a scavenging rate of about 53.75-59.25%; while Comparative Examples 1-5 have significantly poor ability to scavenge DPPH free radicals, with a scavenging rate of less than 21.25%. The data show that the anti-dandruff composition of the present invention can slow down the oxidation of unsaturated fatty acids, triglycerides, cholesterol, etc.; improve the scalp barrier function, and reduce the problems of scalp itching, dryness, and dandruff.
[0135] 3. In vitro test - 5α-reductase activity inhibition test:
[0136] (1) Reagents and instruments
[0137] Reagents: phosphate buffer (pH = 7.2), 150 mg / ml 5α-reductase, 0.5 mg / ml testosterone, 1 mg / ml coenzyme II tetrasodium salt solution, 0.1% finasteride solution;
[0138] Instrument: ELISA reader.
[0139] (2) Test method
[0140] S1: Add 100 μL of 0.5 mg / ml testosterone, 200 μL of phosphate buffer, 15 μL of 1 mg / ml coenzyme II tetrasodium salt solution to the reaction tube, and finally add 15 μL of 150 mg / ml 5α-reductase, mix and incubate at 37°C, and measure the A340nm value after 60 minutes.
[0141] S2: Add 50 μL of 0.1% finasteride solution, 100 μL of 0.5 mg / ml testosterone, 200 μL of phosphate buffer, 15 μL of 1 mg / ml coenzyme II tetrasodium salt solution to the reaction tube, and finally add 15 μL of 150 mg / ml 5α-reductase, mix and incubate at 37°C for 60 min, then measure the A340nm value.
[0142] S3: Add 50 μL of the anti-dandruff shampoo sample solution of Example 1-5 and Comparative Example 1-5, 100 μL of 0.5 mg / ml testosterone, 200 μL of phosphate buffer, 15 μL of 1 mg / ml reduced coenzyme II tetrasodium salt solution, and finally add 15 μL of 150 mg / ml 5α-reductase into the reaction tube, mix and incubate at 37°C for 60 min, and then measure the A340nm value.
[0143] The calculation formula of the 5α-reductase inhibition rate of the sample is:
[0144]
[0145] A1: absorbance of blank control sample; A3: absorbance of sample.
[0146] Table 5 5α-reductase activity inhibition rate
[0147] Sample name Inhibition rate (%) Example 1 43.25 Example 2 45.21 Example 3 45.44 Example 4 43.75 Example 5 47.45 Comparative Example 1 11.85 Comparative Example 2 13.75 Comparative Example 3 8.95 Comparative Example 4 13.35 Comparative Example 5 9.15 Blank control sample 0.5 Finasteride (positive control) 40.65
[0148] It can be seen from Table 5 that the shampoo containing the anti-dandruff composition of Examples 1-5 has an inhibition rate of 5α-reductase activity higher than 43.25%, which is significantly higher than 40.65% of finasteride (positive control sample), while the shampoo containing the anti-dandruff composition of Comparative Examples 1-5 has an inhibition rate of 5α-reductase activity lower than 13.75%, indicating that the anti-dandruff composition of the present invention has the functions of regulating sebum secretion, balancing sebum secretion, reducing hair follicle blockage, improving hair loss, microbial reproduction, and improving the problems of greasy hair, stuffy hair, dryness and itching caused by it.
[0149] It can be seen that the above-mentioned anti-dandruff composition can play a synergistic role by compounding the root of Sophora flavescens, the root of Saposhnikovia divaricata, the bark of Magnolia officinalis, the root of Licorice and the leaf of Andrographis paniculata. Through the synergistic effect, the reproduction and production of Malassezia furfur can be effectively inhibited, thereby reducing the production of dandruff, improving the microbial environment of hair, and restoring the hair to black, bright and smooth. Through the synergistic effect, the activity of 5-α reductase can be inhibited, sebum secretion can be regulated, sebum secretion can be balanced, hair follicle blockage can be reduced, hair loss and microbial reproduction can be improved, and the problems of dry itching caused by greasy hair and airtightness can be improved. Through the synergistic effect, the generation of DPPH free radicals can be effectively removed, the oxidation of unsaturated fatty acids, triglycerides, cholesterol, etc. can be slowed down, the oxidation of secreted oils and fats can be improved, and the inflammation caused by the blockage of scalp oil secretion can be relieved. At the same time, this anti-dandruff composition adopts Chinese medicine ingredients, is safe and non-irritating, can be used for a long time, does not remain, and has obvious effect in improving dandruff.
[0150] The technical features of the above-described embodiments may be arbitrarily combined. To make the description concise, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.
[0151] The specific embodiments described above further describe the purpose, technical solutions and beneficial effects of the present application in detail. It should be understood that the above description is only a specific embodiment of the present application and is not intended to limit the scope of protection of the present application. It is particularly pointed out that for those skilled in the art, any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of protection of the present application.
Claims
1. An anti-dandruff composition, characterized in that: It is composed of the following components in weight percentage: Sophora flavescens root 1%-5%, Saposhnikovia root 0.5%-5%, Magnolia officinalis bark 0.5%-2%, Licorice root 0.3%-2%, Andrographis paniculata leaf 0.1%-1%, and the rest is solvent; The preparation method of the anti-dandruff composition comprises the following steps: Step 1: Weigh the roots of Sophora flavescens, Saposhnikovia divaricata, Magnolia officinalis bark, Licorice root and Andrographis paniculata leaf respectively, crush them into 80-250 mm using a crusher and mix them for later use; Step 2: Weigh the mixture of step 1 and 50% ethanol in a mass ratio of 1:10-50, reflux extract in a constant temperature water bath at 80°C-90°C for 120min-150min, cool naturally to room temperature, and filter to obtain extract I for later use; Step 3: The filter residue of step 2 is mixed with 60% ethanol in a mass ratio of 1:10-50, and reflux extraction is performed in a constant temperature water bath at 80°C-90°C for 120min-150min, and then naturally cooled to room temperature, and filtered to obtain extract II for standby use; Step 4: The filter residue of step 3 is mixed with 70% ethanol in a mass ratio of 1:10-50, and reflux extraction is performed in a constant temperature water bath at 80°C-90°C for 120min-150min, and then naturally cooled to room temperature, and filtered to obtain extract III for standby use; Step 5: Combine the extracts I, II and III, let stand for 12 hours, take the supernatant and add it to a rotary bottle, put it in a rotary evaporator at 85°C to 95°C in a water bath for compression distillation for 120min to 150min, recover ethanol, and cool it naturally to room temperature to obtain concentrated solution IV; Step 6: Add 95% ethanol at a mass ratio of 1:50-70 to the concentrated solution IV in step 5 under stirring with a stirrer, stir for 30 minutes, let stand for 12 hours, take the supernatant after precipitation is complete, add it to a rotary bottle, put it in a rotary evaporator in a water bath at 85°C-95°C for compression distillation for 120min-150min, recover ethanol, and cool it naturally to room temperature to obtain a concentrated solution V; Step 7: Put the concentrated liquid V in step 6 into a beaker, add solvent, heat to 75°C ~ 85°C, weigh the preservative, dissolve it in the container and evenly add it to the beaker, stir at 35r / min ~ 45r / min for 30min ~ 40min, cool to room temperature, put it into a plastic container, put it in a refrigerator at 0°C ~ 5°C and let it stand for 12h. After precipitation is complete, filter with a -0.05MPa ~ -0.1MPa pressure vacuum pump and 800 mesh filter cloth to obtain a clear liquid, i.e., the anti-dandruff composition.
2. The anti-dandruff composition according to claim 1, characterized in that It is composed of the following components in weight percentage: Sophora flavescens root 1%, Saposhnikovia root 5%, Magnolia officinalis bark 2%, Licorice root 1.8%, Andrographis paniculata leaf 0.2%, and the rest are solvents.
3. The anti-dandruff composition according to claim 1 or 2, characterized in that The solvent is composed of components in the following mass ratio: the mass ratio of polyol to deionized water is 1:2-10; the polyol includes one or more of butanediol, isoprenediol, 1,2-ethylene glycol, 1,2-pentanediol and 1,3-propylene glycol.
4. The anti-dandruff composition according to claim 1 or 2, characterized in that The anti-dandruff composition also includes 0.5% to 2% of preservatives.
5. The anti-dandruff composition according to claim 1, characterized in that The preparation method comprises the following steps: Step 1: Weigh the roots of Sophora flavescens, Saposhnikovia divaricata, Magnolia officinalis bark, Licorice root and Andrographis paniculata leaf respectively, crush them into 200 mm using a crusher and mix them for later use; Step 2: Weigh the mixture of step 1 and 50% ethanol in a mass ratio of 1:10, reflux extract in a constant temperature water bath at 90°C for 120 minutes, cool naturally to room temperature, and filter to obtain extract I for later use; Step 3: The filter residue of step 2 was mixed with 60% ethanol in a mass ratio of 1:50, and refluxed in a constant temperature water bath at 88°C for 130 minutes, then naturally cooled to room temperature, and filtered to obtain extract II for later use; Step 4: The filter residue of step 3 was mixed with 70% ethanol in a mass ratio of 1:30, and refluxed in a constant temperature water bath at 82°C for 150 minutes, then naturally cooled to room temperature, and filtered to obtain extract III for later use; Step 5: Combine the extracts I, II and III, let stand for 12 hours, take the supernatant and add it to a rotary bottle, put it in a water bath 85°C rotary evaporator for compression distillation for 150 minutes, recover ethanol, and naturally cool to room temperature to obtain concentrated solution IV; Step 6: Add 95% ethanol at a mass ratio of 1:60 to the concentrated solution IV in step 5 under stirring with a stirrer, stir for 30 minutes, let stand for 12 hours, take the supernatant after precipitation is complete, add it to a rotary bottle, put it in a water bath at 95°C rotary evaporator for compression distillation for 120 minutes, recover ethanol, and naturally cool to room temperature to obtain a concentrated solution V; Step 7: Put the concentrated liquid V in step 6 into a beaker, add solvent, heat to 85°C, weigh the preservative, dissolve it in the container and add it to the beaker, stir at 35r / min for 40min, cool to room temperature, put it into a plastic container, put it in a refrigerator at 2°C and let it stand for 12h. After precipitation is complete, filter with a -0.09MPa pressure vacuum pump and 800 mesh filter cloth to obtain a clear liquid, i.e., the anti-dandruff composition.
6. Use of the anti-dandruff composition according to any one of claims 1 to 5 in the preparation of an anti-dandruff product, characterized in that: The anti-dandruff composition is added in an amount of 1% to 10% in the anti-dandruff product.
7. Use of an anti-dandruff composition according to claim 6 in the preparation of an anti-dandruff product, characterized in that: The anti-dandruff composition is added in an amount of 3% to 10% in the anti-dandruff product.
8. Use of an anti-dandruff composition according to claim 6 in the preparation of an anti-dandruff product, characterized in that: The anti-dandruff and anti-hair loss products include shampoo, hair mask, anti-dandruff water, hair conditioner or hair growth liquid.
Citation Information
Patent Citations
Composition with itching relieving, anti-inflammatory and anti-dandruff functions and preparation method thereof
CN112587460A