Anti-hair-loss and oil-control shampoo and preparation method thereof

Abstract

The invention relates to the technical field of cosmetics, in particular to anti-hair-loss and oil-control shampoo and a preparation method thereof. The hair loss prevention and oil control shampoo is prepared from the following components in parts by weight: 11 to 40 parts of a surfactant, 2 to 20 parts of a platycladus orientalis extract, 0.1 to 0.8 part of a cationic conditioner, 0.05 to 0.2 part of a chelating agent, 0.3 to 1.3 parts of a rheology modifier and 50 to 75 parts of water, the platycladus orientalis extract is prepared from isoquercitrin, afzelin, amentoflavone, pinus koraiensis lactone and dextro-quinic acid in the mass ratio of the isoquercitrin to the afzelin to the amentoflavone to the pinus koraiensis lactone to the dextro-quinic acid being 1 to (2 to 2.7) to (3.5 to 5) to (2 to 2.6) to (650 to 890). Flocculation is generated through the synergistic effect of the platycladus orientalis extract and the cationic conditioner, the composition can be better attached to the scalp, the retention time is prolonged, and the anti-hair-loss and oil-control effects are remarkably improved.

Description

Technical Field

[0001] The invention relates to the technical field of cosmetics, and in particular to an anti-hair loss and oil-control shampoo and a preparation method thereof. Background Art

[0002] With the continuous development of society, people's daily routines, stress levels and eating habits have undergone tremendous changes, and the number of people suffering from hair loss has increased sharply and is becoming younger. Hair loss has not only received attention from the medical community, but has also attracted much attention in the daily chemical industry in recent years. Many well-known brands have launched anti-hair loss and hair growth products, and anti-hair loss and hair growth cosmetics have gradually entered the public eye. In response to such market demand, a large number of cosmetic raw materials claiming to have anti-hair loss and hair growth effects have appeared one after another, among which anti-hair loss shampoo is an important product form of anti-hair loss products.

[0003] Anti-hair loss shampoo is a cleansing product. Its active ingredients need to be in contact with the scalp for a long time to be effective. How to achieve obvious anti-hair loss effects while ensuring product safety is a difficult point in the development of anti-hair loss shampoo.

[0004] In view of this, the present invention is proposed. Summary of the invention

[0005] One object of the present invention is to provide an anti-hair loss and oil control shampoo, which improves the adhesion of active ingredients to the scalp and improves the anti-hair loss and oil control effects through the regulation of components.

[0006] Another object of the present invention is to provide a method for preparing the anti-hair loss and oil-control shampoo.

[0007] In order to achieve the above-mentioned object of the present invention, the present invention provides an anti-hair loss and oil control shampoo on one hand, comprising the following components in parts by weight:

[0008] 11-40 parts of surfactant, 2-20 parts of Platycladus orientalis extract, 0.1-0.8 parts of cationic conditioning agent, 0.05-0.2 parts of chelating agent, 0.3-1.3 parts of rheology modifier and 50-75 parts of water;

[0009] The Platycladus orientalis extract comprises isoquercetin, afusadrin, aconitum biflavonoids, pine lactone and dextrorotatory quinic acid in a mass ratio of 1:(2-2.7):(3.5-5):(2-2.6):(650-890).

[0010] In a specific embodiment of the present invention, in the Platycladus orientalis extract, the percentages of isoquercetin, afudamidin and aconitum biflavonoids in the total flavonoids are 0.30% to 1.00%, 0.60% to 1.90% and 3.50% to 3.90% respectively.

[0011] In a specific embodiment of the present invention, the Platycladus orientalis extract further comprises at least one of propylene glycol and butylene glycol.

[0012] In a specific embodiment of the present invention, the Platycladus orientalis extract further comprises PEG-40 hydrogenated castor oil and / or disodium EDTA. Further, in the Platycladus orientalis extract, the mass fraction of the PEG-40 hydrogenated castor oil is 0.2% to 0.6%, and the mass fraction of the disodium EDTA is 0.1% to 0.2%.

[0013] In a specific embodiment of the present invention, the preparation of the Platycladus orientalis extract comprises:

[0014] (a) using ethanol aqueous solution as the extraction solvent, with a solid-liquid ratio of 1:10 to 1:30, and extracting Platycladus orientalis leaves at 25 to 85°C for 1 to 3 hours;

[0015] (b) adjusting the pH of the extract obtained by the extraction to 8.3-9.5, stirring the extract, filtering the extract, and then adjusting the pH to 7.0±0.5.

[0016] In a specific embodiment of the present invention, the preparation of the Platycladus orientalis extract further comprises: concentrating the material adjusted to pH 7.0±0.5, and re-dissolving it with a propylene glycol aqueous solution or a butylene glycol aqueous solution. Further, adding PEG-40 hydrogenated castor oil and / or disodium EDTA to the re-dissolved material.

[0017] In a particular embodiment of the present invention, the cationic conditioning agent includes at least one of guar hydroxypropyltrimonium chloride, polyquaternium-10, and polyquaternium-39.

[0018] In a specific embodiment of the present invention, the mass ratio of the Platycladus orientalis extract to the cationic conditioning agent is (20-35) : 1, preferably (30-35) : 1.

[0019] In a specific embodiment of the present invention, the anti-hair loss and oil control shampoo further comprises a pH regulator and / or a preservative. Further, the anti-hair loss and oil control shampoo further comprises the following components by weight: 0.01 to 0.1 parts of a pH regulator and 0.1 to 1 parts of a preservative.

[0020] Another aspect of the present invention provides a method for preparing any one of the above-mentioned anti-hair loss and oil-control shampoos, comprising the following steps: mixing the components in proportion.

[0021] In a specific embodiment of the present invention, the following steps are included:

[0022] (A) mixing water, a chelating agent and a cationic conditioning agent in proportion and dissolving them, then adding a surfactant, heating to 80-85° C. and stirring until dissolved;

[0023] (B) Cooling the material obtained in step (A) to below 45°C, adding the remaining materials and stirring evenly.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] (1) In the anti-hair loss and oil control shampoo of the present invention, the arborvitae extract and the cationic conditioning agent work synergistically, so that the arborvitae extract can flocculate with the cationic conditioning agent, better adhere to the scalp, prolong the residence time, and significantly improve the anti-hair loss and oil control effect;

[0026] (2) The preparation method of the anti-hair loss and oil control shampoo of the present invention is simple to operate, and the prepared shampoo has good stability and use feeling. DETAILED DESCRIPTION

[0027] The technical scheme of the present invention will be clearly and completely described below in conjunction with specific embodiments, but it will be appreciated by those skilled in the art that the following described embodiments are part of embodiments of the present invention, rather than all embodiments, and are only used to illustrate the present invention, and should not be considered as limiting the scope of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative work, all belong to the scope of protection of the present invention. If specific conditions are not indicated in the embodiments, they are carried out according to normal conditions or conditions recommended by the manufacturer. If the manufacturer is not indicated in the reagents or instruments used, they are all conventional products that can be purchased commercially.

[0028] In one aspect, the present invention provides an anti-hair loss and oil control shampoo, comprising the following components in parts by weight:

[0029] 11-40 parts of surfactant, 2-20 parts of Platycladus orientalis extract, 0.1-0.8 parts of cationic conditioning agent, 0.05-0.2 parts of chelating agent, 0.3-1.3 parts of rheology modifier and 50-75 parts of water;

[0030] The Platycladus orientalis extract includes isoquercetin, afusadrin, sedum flavonoids, pinolactone and dextrorotatory quinic acid in a mass ratio of 1:(2-2.7):(3.5-5):(2-2.6):(650-890).

[0031] In the anti-hair loss and oil-control shampoo of the present invention, through the synergistic effect of the Platycladus orientalis extract and the cationic conditioning agent, the Platycladus orientalis extract can flocculate with the cationic conditioning agent, better adhere to the scalp, prolong the residence time, and significantly improve the anti-hair loss and oil-control effect.

[0032] For example, in different embodiments, the amount of each component in the anti-hair loss and oil control shampoo can be as follows in parts by weight:

[0033] The amount of the surfactant can be 11 parts, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts or a range consisting of any two of them;

[0034] The amount of the Platycladus orientalis extract can be 2 parts, 5 parts, 8 parts, 10 parts, 12 parts, 15 parts, 18 parts, 20 parts or a range consisting of any two of them;

[0035] The amount of the cationic conditioning agent can be 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part or a range consisting of any two thereof;

[0036] The amount of the chelating agent can be 0.05 parts, 0.1 parts, 0.15 parts, 0.2 parts or a range consisting of any two of them;

[0037] The amount of the rheology modifier can be 0.3 parts, 0.5 parts, 0.8 parts, 1 part, 1.3 parts or a range consisting of any two thereof;

[0038] The amount of water can be 50 parts, 55 parts, 60 parts, 65 parts, 70 parts, 75 parts or a range consisting of any two of them.

[0039] In the Platycladus orientalis extract, the mass ratios of afudamidin, aconitum biflavonoids, koreanolide and dextrorotatory quinic acid to isoquercetin can be exemplified as follows:

[0040] The mass ratio of afudamirin to isoquercetin can be 2, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7 or a range consisting of any two thereof;

[0041] The mass ratio of aconitum biflavonoids to isoquercetin can be 3.5, 3.8, 4, 4.2, 4.5, 4.8, 5 or a range consisting of any two thereof;

[0042] The mass ratio of koreanolide to isoquercetin may be 2, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6 or a range consisting of any two of them;

[0043] The mass ratio of dextrorotatory quinic acid to isoquercetin can be 650, 660, 680, 700, 750, 800, 850, 890 or a range consisting of any two of them.

[0044] In a specific embodiment of the present invention, in the Platycladus orientalis extract, the percentages of isoquercetin, afudamidin and aconitum biflavonoids in the total flavonoids are 0.30% to 1.00%, 0.60% to 1.90% and 3.50% to 3.90% respectively.

[0045] For example, in different embodiments, in the Platycladus orientalis extract, the percentage of isoquercetin in the total flavonoids can be 0.3%, 0.4%, 0.5%, 0.6%, 0.8%, 1% or a range consisting of any two thereof; the percentage of afudamidin in the total flavonoids can be 0.6%, 0.8%, 1%, 1.2%, 1.5%, 1.8%, 1.9% or a range consisting of any two thereof; the percentage of aconitum biflavonoids in the total flavonoids can be 3.5%, 3.6%, 3.7%, 3.8%, 3.9% or a range consisting of any two thereof. Total flavonoids refers to all flavonoid components in the Platycladus orientalis extract.

[0046] In a specific embodiment of the present invention, the Platycladus orientalis extract further comprises at least one of propylene glycol and butylene glycol. Propylene glycol may comprise 1,2-propylene glycol and / or 1,3-propylene glycol; butylene glycol comprises at least one of 1,2-butylene glycol, 1,3-butylene glycol and 1,4-butylene glycol.

[0047] In a specific embodiment of the present invention, the Platycladus orientalis extract further comprises PEG-40 hydrogenated castor oil and / or disodium EDTA. Further, in the Platycladus orientalis extract, the mass fraction of PEG-40 hydrogenated castor oil is 0.2% to 0.6%, and the mass fraction of disodium EDTA is 0.1% to 0.2%.

[0048] For example, in different embodiments, in the Platycladus orientalis extract, the mass fraction of PEG-40 hydrogenated castor oil can be 0.2%, 0.3%, 0.4%, 0.5%, 0.6% or a range consisting of any two thereof, and the mass fraction of disodium EDTA can be 0.1%, 0.12%, 0.15%, 0.18%, 0.2% or a range consisting of any two thereof.

[0049] In a specific embodiment of the present invention, the preparation of the Platycladus orientalis extract comprises:

[0050] (a) using ethanol aqueous solution as the extraction solvent, with a solid-liquid ratio of 1:10 to 1:30, and extracting Platycladus orientalis leaves at 25 to 85°C for 1 to 3 hours;

[0051] (b) The pH of the extract obtained by extraction is adjusted to 8.3-9.5, and after stirring, the extract is finely filtered and then the pH is adjusted to 7.0±0.5.

[0052] The extract obtained by extracting Platycladus orientalis leaves contains a large amount of tannins, which will affect the stability of the system. The impurity removal method of the present invention can effectively remove the tannins therein, significantly reduce the turbidity of the system, and make it easy to filter after impurity removal; at the same time, the impurity removal process will retain the tannic acid substance dextrorotatory quinic acid in the system, which can achieve selective impurity removal, thereby increasing the content of active ingredients in the extract.

[0053] For example, in different embodiments, in the preparation method, each parameter can be exemplified as follows: the solid-liquid ratio can be 1:10, 1:12, 1:15, 1:18, 1:20, 1:22, 1:25, 1:28, 1:30 or a range consisting of any two thereof; the extraction temperature can be 25°C, 30°C, 35°C, 40°C, 45°C, 50°C, 55°C, 60°C, 65°C, 70°C, 75°C, 80°C or a range consisting of any two thereof; the extraction time can be 1h, 1.5h, 2h, 2.5h, 3h or a range consisting of any two thereof.

[0054] Sodium hydroxide and / or citric acid can be used to adjust the pH. The specific form of sodium hydroxide and / or sodium citrate is not limited, such as aqueous solution, the mass fraction of the aqueous solution can be 10%, 20%, etc., but not limited thereto.

[0055] In a specific embodiment of the present invention, the volume fraction of ethanol in the ethanol aqueous solution is 50% to 80%, preferably 50% to 60%.

[0056] For example, in different embodiments, the volume fraction of ethanol in the ethanol aqueous solution can be 50%, 55%, 60%, 65%, 70%, 75%, 80% or a range consisting of any two thereof.

[0057] In a specific embodiment of the present invention, Platycladus orientalis leaves are extracted in a coarse powder state, and the particle size of the coarse powder is above a 50-mesh sieve.

[0058] The present invention has found in the research that if the particle size of the raw material to be extracted is too small, it will lead to difficulty in filtering, large loss of active ingredients, and too dark color of the finished product. Through research, it is known that on the coarse powder particle size 50 mesh sieve, it can ensure the effective extraction of active ingredients and reduce the loss of active ingredients during the filtration process.

[0059] In a specific embodiment of the present invention, the preparation of the Platycladus orientalis extract further comprises: concentrating the material adjusted to pH 7.0±0.5, and re-dissolving it with a propylene glycol aqueous solution or a butylene glycol aqueous solution. Further, adding PEG-40 hydrogenated castor oil and / or disodium EDTA to the re-dissolved material.

[0060] In a specific embodiment of the present invention, the amount of the propylene glycol aqueous solution or the butylene glycol aqueous solution is 4 to 12 times the weight of the crude drug.

[0061] For example, in different embodiments, based on the amount of crude drug, the amount of propylene glycol aqueous solution or butylene glycol aqueous solution can be 4 times, 5 times, 6 times, 7 times, 8 times, 9 times, 10 times, 11 times, 12 times the weight of the crude drug, or a range consisting of any two of them.

[0062] In a specific embodiment of the present invention, in the propylene glycol aqueous solution, the mass fraction of propylene glycol is 20% to 40%; in the butylene glycol aqueous solution, the mass fraction of butylene glycol is 20% to 60%.

[0063] For example, in different embodiments, in the propylene glycol aqueous solution, the mass fraction of propylene glycol can be 20%, 25%, 30%, 35%, 40% or a range consisting of any two thereof; in the butylene glycol aqueous solution, the mass fraction of butylene glycol can be 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60% or a range consisting of any two thereof.

[0064] In actual operation, the re-dissolution includes: adding propylene glycol aqueous solution or butylene glycol aqueous solution, stirring, and fine filtering.

[0065] In a particular embodiment of the present invention, the cationic conditioning agent includes at least one of guar hydroxypropyltrimonium chloride, polyquaternium-10, and polyquaternium-39.

[0066] In a specific embodiment of the present invention, the mass ratio of the Platycladus orientalis extract to the cationic conditioning agent is (20-35) : 1, such as (30-35) : 1.

[0067] By adjusting the mass ratio of the Platycladus orientalis extract to the cationic conditioning agent within the above range, the anti-hair loss and oil control effects are further improved. For example, in different embodiments, the mass ratio of the Platycladus orientalis extract to the cationic conditioning agent can be 20:1, 22:1, 25:1, 28:1, 30:1, 32:1, 35:1 or any two thereof.

[0068] In a specific embodiment of the present invention, the anti-hair loss and oil control shampoo further comprises a pH regulator and / or a preservative. Further, the anti-hair loss and oil control shampoo further comprises the following components by weight: 0.01 to 0.1 parts of a pH regulator and 0.1 to 1 parts of a preservative.

[0069] In a specific embodiment of the present invention, the surfactant includes the following components by weight: 10 to 25 parts of a main surfactant and 1 to 15 parts of an auxiliary surfactant. Further, the main surfactant includes sodium laureth sulfate and / or ammonium laureth sulfate; the auxiliary surfactant includes at least one of lauryl hydroxysulfobetaine, cocamidopropyl betaine, sodium cocoamphoacetate and cocamide MEA.

[0070] For example, in different embodiments, among the surfactants, the amount of the main surfactant can be 10 parts, 12 parts, 15 parts, 18 parts, 20 parts, 22 parts, 25 parts or a range consisting of any two thereof, and the amount of the auxiliary surfactant can be 1 part, 2 parts, 5 parts, 8 parts, 10 parts, 15 parts or a range consisting of any two thereof, by weight.

[0071] In a specific embodiment of the present invention, the chelating agent includes at least one of disodium EDTA, trisodium EDTA, tetrasodium EDTA and sodium glucoheptonate.

[0072] In a specific embodiment of the present invention, the rheology modifier includes at least one of sodium chloride, trihydroxystearin, carbomer 2020, acrylic copolymer, trihydroxystearin, ammonium xylene sulfonate, polyethylene glycol-14M and silica.

[0073] In a specific embodiment of the present invention, the pH adjuster includes at least one of citric acid, sodium citrate and sodium hydroxide.

[0074] In a specific embodiment of the present invention, the preservative includes at least one of phenoxyethanol, ethylhexylglycerin, chlorphenesin, methylchloroisothiazolinone, methylisothiazolinone and sodium benzoate.

[0075] Another aspect of the present invention provides a method for preparing any one of the above-mentioned anti-hair loss and oil-control shampoo, comprising the following steps: mixing the components in proportion.

[0076] In a specific embodiment of the present invention, the following steps are included:

[0077] (A) mixing water, a chelating agent and a cationic conditioning agent in proportion and dissolving them, then adding a surfactant, heating to 80-85° C. and stirring until dissolved;

[0078] (B) Cooling the material obtained in step (A) to below 45°C, adding the remaining materials and stirring evenly.

[0079] Examples 1 to 3

[0080] Examples 1 to 3 provide anti-hair loss and oil control shampoos, respectively, and their raw materials and amounts are shown in Table 1.

[0081] Table 1 Formula of the anti-hair loss and oil control shampoo of Examples 1 to 3

[0082]

[0083] Note: The mass ratio of phenoxyethanol to ethylhexylglycerin is 9:1, and the mass ratio of methylchloroisothiazolinone to methylisothiazolinone is 3:1.

[0084] The preparation method of the oil-control shampoo of Examples 1 to 3 comprises the following steps:

[0085] (1) Stir the raw materials of phase A until they are completely dissolved;

[0086] (2) Add the raw materials of phase B to the materials of step (1) in sequence, heat to 80-85° C. and stir until completely dissolved;

[0087] (3) Cooling the material obtained in step (2) to below 45° C., then adding the raw materials of phase C in sequence and stirring thoroughly;

[0088] (4) The material obtained in step (3) is cooled to below 38° C. and discharged after being inspected and found to be qualified.

[0089] The preparation method of the Platycladus orientalis extract in Examples 1 to 3 comprises the following steps:

[0090] (1) Crush the Platycladus orientalis leaves, take the material on a 10-mesh sieve, use a 50% by volume ethanol aqueous solution as an extraction solvent, add the extraction solvent at a solid-liquid ratio of 1:15 (m / V), and soak for 0.5 h; then extract at 85°C for 1 h, and coarsely filter the extracted material to obtain an extract.

[0091] (2) The extract obtained in step (1) is adjusted to a pH of 9.3 to 9.5, stirred for 0.5 h to remove impurities, and then finely filtered to control the turbidity to ≤ 3, and the fine filtrate is collected; the pH of the fine filtrate is adjusted to 7.0 ± 0.1.

[0092] (3) The material obtained in step (2) is concentrated until the amount of crude drug reaches ±5%, and a 20% by mass fraction of 1,3-propylene glycol aqueous solution is added according to 9 times the amount of crude drug for redissolution, mechanically stirred at room temperature for 30 minutes, and 0.5% PEG-40 hydrogenated castor oil (the mass fraction of PEG-40 hydrogenated castor oil in the whole solution is 0.5%) is added for solubilization; then 0.1% (the mass fraction of disodium EDTA in the product) of disodium EDTA is added for color protection, and a clear solution is obtained by filtering; and then sterilized at 85° C. for 40 minutes to obtain a Platycladus orientalis extract.

[0093] Example 4

[0094] This embodiment refers to the anti-hair loss and oil control shampoo and preparation method thereof of Example 1, the only difference being that different amounts of cationic conditioning agents and water are used.

[0095] In this embodiment, the addition amount of guar hydroxypropyltrimethylammonium chloride is 0.4%, and the addition amount of water is 63.85%.

[0096] Example 5

[0097] This embodiment refers to the anti-hair loss and oil control shampoo and preparation method thereof of Example 1, the only difference being that different amounts of cationic conditioning agents and water are used.

[0098] In this embodiment, the addition amount of guar hydroxypropyltrimethylammonium chloride is 0.2%, and the addition amount of water is 62.05%.

[0099] Example 6

[0100] This example refers to the anti-hair loss and oil-control shampoo and preparation method thereof of Example 1, with the only difference being that different amounts of Platycladus orientalis extract and water are used.

[0101] In this example, the amount of the Platycladus orientalis extract added is 7.5%, and the amount of water added is 64.45%.

[0102] Example 7

[0103] This example refers to the anti-hair loss and oil-control shampoo and preparation method thereof of Example 1, with the only difference being that different amounts of Platycladus orientalis extract and water are used.

[0104] In this example, the amount of the Platycladus orientalis extract added is 15%, and the amount of water added is 56.95%.

[0105] Comparative Examples 1 to 5

[0106] Comparative Examples 1 to 5 refer to the shampoo and preparation method of Example 1, except that the raw materials and amounts are different. The raw materials and amounts of Comparative Examples 1 to 5 are shown in Table 2.

[0107] Table 2 Formulas of shampoos of Comparative Examples 1 to 5

[0108]

[0109] Among them, the Platycladus orientalis extract A is the same as the Platycladus orientalis extract in Example 1.

[0110] Platycladus orientalis extract B is: a commercially available competitor, a certain brand of Platycladus orientalis leaf extract, the main ingredients of which include: propylene glycol, water, Platycladus orientalis (BIOTA ORIENTALIS) leaf extract, phenoxyethanol, and ethylhexylglycerin.

[0111] Comparative Example 6

[0112] Comparative Example 6 refers to the anti-hair loss and oil-control shampoo and preparation method thereof of Example 1, except that a different Platycladus orientalis extract is used.

[0113] The preparation method of the Platycladus orientalis extract of Comparative Example 6 comprises the following steps:

[0114] (1) Crush the Platycladus orientalis leaves, take the material on a 10-mesh sieve, use a 50% by volume ethanol aqueous solution as an extraction solvent, add the extraction solvent at a solid-liquid ratio of 1:15 (m / V), and soak for 0.5 h; then extract at 85°C for 1 h, and coarsely filter the extracted material to obtain an extract.

[0115] (2) The material obtained in step (1) is concentrated until the amount reaches ±5% of the crude drug amount, and a 20% by mass fraction of 1,3-propylene glycol aqueous solution is added according to 9 times the amount of the crude drug for redissolution, mechanically stirred at room temperature for 30 minutes, and 0.5% PEG-40 hydrogenated castor oil (the mass fraction of PEG-40 hydrogenated castor oil in the whole solution is 0.5%) is added for solubilization; then 0.1% (the mass fraction of disodium EDTA in the product) of disodium EDTA is added for color protection, and a clear solution is obtained by filtering; and then sterilized at 85° C. for 40 minutes to obtain a Platycladus orientalis extract.

[0116] Comparative Example 7

[0117] Comparative Example 7 refers to the anti-hair loss and oil-control shampoo and preparation method thereof of Example 1, the only difference being that a different Platycladus orientalis extract is used.

[0118] The preparation method of the Platycladus orientalis extract of Comparative Example 7 comprises the following steps:

[0119] (1) Crush Platycladus orientalis leaves into fine powder (under 30 mesh sieve, on 50 mesh sieve), add 50% by volume ethanol aqueous solution as extraction solvent at a solid-liquid ratio of 1:15 (m / V), and soak for 0.5 h; then extract at 85°C for 1 h, and coarsely filter the extracted material to obtain an extract.

[0120] (2) The extract obtained in step (1) is adjusted to a pH of 9.3 to 9.5, stirred for 0.5 h to remove impurities, and then finely filtered to control the turbidity to ≤ 3, and the fine filtrate is collected; the pH of the fine filtrate is adjusted to 7.0 ± 0.1.

[0121] (3) The material obtained in step (2) is concentrated until the amount of crude drug reaches ±5%, and a 20% by mass fraction of 1,3-propylene glycol aqueous solution is added according to 9 times the amount of crude drug for redissolution, mechanically stirred at room temperature for 30 minutes, and 0.5% PEG-40 hydrogenated castor oil (the mass fraction of PEG-40 hydrogenated castor oil in the whole solution is 0.5%) is added for solubilization; then 0.1% (the mass fraction of disodium EDTA in the product) of disodium EDTA is added for color protection, and a clear solution is obtained by filtering; and then sterilized at 85° C. for 40 minutes to obtain a Platycladus orientalis extract.

[0122] Experimental Example 1

[0123] The composition of the Platycladus orientalis extract used in Example 1 and Comparative Example 6 was analyzed. Since the Platycladus orientalis extract used in Example 1 and Comparative Example 6 is a liquid, and contains additional components such as a reconstitution solvent, PEG-40, and disodium EDTA, in order to reduce interference with component detection, the material obtained in step (2) of the preparation of the Platycladus orientalis extract in Example 1 and the material obtained in step (1) of the preparation of the Platycladus orientalis extract in Comparative Example 6 were processed into solid powders, and then the full component analysis was performed and the percentage of flavonoids in the total flavonoids was detected to reduce interference.

[0124] The method for processing into solid powder includes: concentrating the corresponding material at 60±5℃ under negative pressure to remove ethanol until the solid content of the concentrate reaches 8% to 10%; placing the concentrate in a spray dryer, controlling the inlet temperature to 140℃, drying for about 1h, collecting the powder, and conducting subsequent testing. Among them, the full component analysis is identified using HPLC-MS / MS (high performance liquid chromatography mass spectrometry). The test results are shown in Tables 3 and 4.

[0125] Table 3 Full component analysis results of Example 1 and Comparative Example 6 (mg / g)

[0126] serial number Isoquercetin Afudamicin Aconitum biflavonoids rosinol D-quinic acid Example 1 0.850 1.925 3.981 1.834 560.61 Comparative Example 6 0.321 1.203 3.320 0.120 709.44

[0127] Table 4 The percentage of flavonoids in Example 1 and Comparative Example 6 in total flavonoids

[0128] serial number Isoquercetin Afudamicin Aconitum biflavonoids Example 1 0.80％ 1.82％ 3.76％ Comparative Example 6 0.35％ 1.31％ 3.60％

[0129] For the convenience of testing, the solid powder corresponding to Example 1 prepared by the above method (i.e., the solid powder sample of full component analysis) was subjected to 5α-reductase inhibition test, Malassezia inhibition test and zebrafish embryo blood circulation promotion efficacy test. The test methods and results are as follows.

[0130] 5α-Reductase Inhibition Assay

[0131] (1) Test drug: solid powder corresponding to Example 1 prepared by the above method.

[0132] (2) Positive control drug: finasteride, a product of Merck Sharp & Dohme Limited; Properties: film-coated tablets, white after removal of the coating; Specification: 5 mg / tablet; Batch number: 0022050. Storage conditions: light-shielded, airtight, and stored at room temperature.

[0133] (3) Drug preparation: The test drug was tested at 10 concentrations: 35 mg / mL (solute is the solid powder of Example 1, solvent is 20% ethanol aqueous solution) was used as the initial concentration, and 9 2.5-fold gradient dilutions were made using 20% ​​ethanol aqueous solution; the positive control finasteride was diluted 5 times by 2 using anhydrous ethanol.

[0134] (4) Reagents: reduced coenzyme II (NADPH), product of Sigma, catalog number N7505, batch number: 041939; testosterone (T), product of Merck, catalog number T-037, batch number: FE03112002; Tris buffer: Shanghai Yuanye Biotechnology Co., Ltd., batch number J17HR10516A.

[0135] (5) Testing instrument: ZDN microplate reader, product of BioTek.

[0136] Test method:

[0137] Mouse liver was dissected and homogenized by adding Tris buffer at a ratio of 1:5 at 0°C, centrifuged at 4°C and 10,000 g for 15 minutes, and the supernatant was centrifuged at 0°C and 55,000 g for 1 hour and then taken out and placed at 4°C for later use. Reagents and samples were added according to the reaction system. Example 1 Solid powder and finasteride samples of each dilution were added 4 times. After incubation at 37°C for 60 minutes, the decrease in absorbance at 340 nm was measured.

[0138]

[0139] The 5α-reductase reaction system is shown in Table 5:

[0140] Table 5 Reagent dosage of reaction system (μL)

[0141] Substance name Addition volume μL Final concentration μmol / L 5α-Reductase Solution 10 - T 5 25 NADPH 10 100 Drugs to be tested 5 PBS 220

[0142] Test results:

[0143] Inhibition rate and IC of 5α-reductase in different concentration gradients of finasteride and tested drugs 50 The results are shown in Table 6.

[0144] Table 6 Inhibition rate and IC of 5α-reductase of the tested drugs and finasteride in Example 1 50

[0145]

[0146]

[0147] From the above results, it can be seen that the Platycladus orientalis extract of Example 1 has an inhibitory effect on the activity of 5α-reductase, IC50 The IC value of Platycladus orientalis extract in the reaction system was 3.78 mg / mL. 50 The concentration of the crude drug is 0.076 mg / mL, which is equivalent to 0.72 mg / mL. In summary, the solid powder of Example 1 of the Platycladus orientalis extract of the present invention has a significant 5α-reductase inhibitory effect at a low concentration.

[0148] Malassezia antibacterial test

[0149] Test Materials:

[0150] (1) Experimental instruments

[0151] The main instruments used in this experiment are shown in Table 7.

[0152] Table 7 Main instruments of the experiment

[0153] Instrument Name model Manufacturer ELISA reader infinite M200 PRO Tecan Centrifuge Centrifuge 5430 R Eppendorf Ultra clean workbench / /

[0154] (2) Experimental reagents

[0155] The main reagents used in this experiment are shown in Table 8.

[0156] Table 8 Main reagents for the experiment

[0157] Reagent name Manufacturer Malt extract medium Obostar Sterile PBS Gibco

[0158] (3) Sample information table

[0159] The sample information of this experiment is shown in Table 9.

[0160] Table 9 Experimental sample information

[0161]

[0162] Note: The solid powder of Comparative Example 7 is prepared using the material obtained in step (2) during the preparation of Platycladus orientalis extract in Comparative Example 7 as raw material.

[0163] Test method:

[0164] Cultivation of Malassezia

[0165] Shake the culture medium and Malassezia until there is no sediment at the bottom. Use a sterile syringe to transfer 200-800 μL of bacterial solution into the new culture medium and culture it in a biochemical incubator at 38°C. After 2-3 days of culture, subculture.

[0166] Micro-broth method to test the antibacterial activity of samples

[0167] 1. Prepare fresh culture medium

[0168] Transfer the sterile malt extract medium into a sterile 50 mL centrifuge tube. Centrifuge the sterile malt extract medium for 10 min at 25°C and 3500 rpm. Take the supernatant and place it in another sterile 50 mL centrifuge tube for later use.

[0169] Each sample was diluted with fresh culture medium to 50 mg / mL, 40 mg / mL, 30 mg / mL, 20 mg / mL, 10 mg / mL, and 5 mg / mL.

[0170] 2. Extraction of Malassezia

[0171] Gently shake the culture medium and Malassezia, transfer to a sterile 50 mL centrifuge tube, centrifuge at 25°C and 1000 rpm for 30 seconds, transfer the supernatant to a sterile 50 mL centrifuge tube, and centrifuge at 25°C and 3500 rpm for 10 minutes.

[0172] 3. Determination of bacterial solution concentration

[0173] Turn on the microplate reader and set the wavelength to 600nm. Take 400μL of the bacterial solution and place it in a 1.5mL sterile centrifuge tube. Add 1mL PBS and take 200μL of the bacterial solution from the 1.5mL centrifuge tube containing 400μL of bacterial solution and place it in a regular 96-well plate. Measure the OD of the bacterial solution at 600nm. 600 If OD 600 When the OD value is > 1, dilute with sterile PBS. (You can explore from 2 times, 4 times, 6 times, and 8 times) When the OD value is equal to 1, you can proceed to the next step of the experiment.

[0174] 4. Dilution of bacterial solution

[0175] Calculate the volume of bacterial suspension required. 600 =1) Dilute 160 times with fresh culture medium.

[0176] 5. Paving

[0177] In a sterile 96-well culture plate, add 100 μL of diluted bacterial suspension to each test well, then add 100 μL of samples of different concentrations, 100 μL of samples of different concentrations + 100 μL of malt medium as the control group, 200 μL of malt medium without bacteria as the blank control, 100 μL of diluted bacterial suspension + 100 μL of malt medium as the negative control, 100 μL of diluted bacterial suspension + 100 μL of 4 μg / mL ketoconazole as the positive control, and make 3 duplicate wells for each.

[0178] A sterile 96-well culture plate was placed in a 38°C incubator. After 72 hours of incubation, the absorbance was measured at 600 nm.

[0179] 6. Malassezia inhibition rate

[0180]

[0181]

[0182] Test results: See Table 10.

[0183] Table 10 Test results

[0184]

[0185]

[0186] From the above results, it can be seen that the solid powder samples of Comparative Examples 6 and 7 have no Malassezia inhibitory effect at a concentration below 50 mg / mL, and the solid powder sample of Example 1 has a Malassezia inhibitory effect at a concentration above 10 mg / mL. In summary, the Platycladus orientalis extract of Example 1 has a significant Malassezia inhibitory effect at a low concentration.

[0187] Zebrafish embryos promote blood circulation

[0188] Test method:

[0189] Pick healthy 3-day-post-fertilization (DPF) zebrafish embryos.

[0190] 1. Test grouping:

[0191] The test requires setting up a blank control group (fish embryo culture medium / solvent solution), a positive control group (caffeine solution) and a test substance group (solid powder sample corresponding to Example 1).

[0192] 2. Blank control group setting:

[0193] 40 fish embryos were randomly selected, transferred to a 6 cm culture dish, and 8 mL of fish embryo culture medium was added.

[0194] 3. Positive control group setting:

[0195] 40 fish embryos were randomly selected and transferred to a 6 cm culture dish, and 8 mL of 0.05 g / L caffeine solution was added (the working solution was 0.05 g / L caffeine solution prepared with fish embryo culture medium).

[0196] 4. Handling of test substances:

[0197] 40 fish embryos were randomly selected and transferred to a 6 cm culture dish, and 8 mL of the test substance solution was added (the test substance was directly dissolved in the fish embryo culture medium to prepare the test solution). The dish was placed in a 28±1°C incubator and cultured for 2±0.5 h.

[0198] 5. Microscopic analysis of samples:

[0199] Use tricaine working solution (weigh 200 mg tricaine (analytical grade) and dissolve it in 48.95 mL water to prepare the storage solution. Refrigerate. It is valid within 30 days. The working solution is diluted to 0.04% with fish embryo culture medium and freshly prepared before use) to anesthetize the fish embryo for 2 minutes, and the dorsal aorta of the fish embryo is photographed for 20 seconds under a microscope.

[0200] 6. Data and result calculation:

[0201] Use software such as DanioScope to measure the relative blood flow velocity in the dorsal aorta of each fish embryo and take the average value.

[0202] Calculation results:

[0203] Calculate the blood circulation promotion rate: promotion rate = (TC) / C×100%;

[0204] In the above formula:

[0205] T—the average relative velocity of blood flow in the dorsal aorta of fish embryos in the test substance treatment group;

[0206] C—The average relative velocity of blood flow in the dorsal aorta of fish embryos in the blank control group.

[0207] A two-tailed T test was performed on the relative blood flow velocity of the dorsal aorta of fish embryos in the test substance treatment group and the relative blood flow of the dorsal aorta of the blank control group to obtain the p value.

[0208] Test results: The test results are shown in Table 11.

[0209] Table 11 Test results

[0210]

[0211]

[0212] From the above results, it can be seen that the solid powder corresponding to Example 1 of the present invention has a significant effect of promoting blood circulation at low concentrations, which to a certain extent proves that the Platycladus orientalis extract of Example 1 has a nourishing and anti-hair loss effect.

[0213] Experimental Example 2

[0214] During the preparation of shampoo products, if the raw materials are not dissolved after stirring for more than 2 hours, it means that this formula cannot be converted into a finished product. After the production is completed, observe the offline status and then test its performance. Observe whether the offline products have unstable phenomena such as stratification, precipitation, too thin or too thick. If not, the status is good; if the product is too thin or too thick, without stratification or precipitation, the status is average; if the product has stratification or precipitation, the status is poor. Then take an appropriate amount of shampoo for shampooing test to examine its cleaning power and the feeling of use during shampooing. The cleaning power is judged as strong, strong, average, weak, and weak. The feeling of use is judged as good, good, average, poor, and poor.

[0215] The preparation feasibility and shampoo test results of the shampoo products of different embodiments and comparative examples are shown in Table 12.

[0216] Table 12 Preparation feasibility and shampoo test results of different shampoo products

[0217]

[0218]

[0219] The experiment found that in Comparative Example 2, due to the high content of guar gum hydroxypropyltrimethylammonium chloride, the dissolution of sodium laureth sulfate was affected, and it was not completely dissolved in 2 hours, so the process was not feasible; in Comparative Example 4, since the Platycladus orientalis extract occupied a large amount of water, the content of water for dissolving sodium laureth sulfate was less, and it was still not completely dissolved in 2 hours, so the formula was not feasible.

[0220] Experimental Example 3

[0221] 1. Comparison of oil control effects

[0222] 60 volunteers (18-55 years old, both male and female) were selected for scalp oil test. The volunteers did not wash their hair the night before the test. The test time points were before sample application, immediately after sample application, and 8 hours after sample application. The test site was the temporal part of the top of the head. The test sample was used to wash the hair. The oil content was tested three times at the test site for analysis. When washing the hair, the same person used the same method to wash the volunteers' hair and used a hair dryer with medium-speed hot air until the volunteers' hair was dry. The volunteers went to the constant temperature and humidity chamber (((22±1)℃, (50±5)%)) 30 minutes before the test time and sat quietly waiting for the measurement. The test results are shown in Table 13.

[0223] Table 13 Scalp oil content at different time periods after using the sample (ug / cm 2 , n=20)

[0224]

[0225]

[0226] From the above test results, it can be seen that Example 1 has a better oil control effect. Compared with Comparative Example 1, Example 1 adds 0.3% more guar hydroxypropyl trimethyl ammonium chloride, which shows that guar hydroxypropyl trimethyl ammonium chloride and Platycladus orientalis extract work together to produce a better synergistic oil control effect. Compared with Comparative Example 5, Example 1 uses a different type of Platycladus orientalis extract, which further shows that the Platycladus orientalis extract in Example 1 is extracted using a special process and has a better long-term oil control effect when combined with guar hydroxypropyl trimethyl ammonium chloride.

[0227] 2. Comparison of anti-hair loss effects

[0228] Volunteer recruitment: Volunteers with hair loss problems will be recruited and screened. They should not wash their hair within 48 hours before each data feedback during the screening and trial period.

[0229] Sample distribution: Staff randomly distribute samples to volunteers and explain the usage and precautions. Volunteers use according to product requirements (after thoroughly wet the hair, take an appropriate amount of the product and rub it on the palm to make bubbles, then apply it to the scalp and hair and massage gently, and finally rinse it thoroughly with clean water).

[0230] Follow-up visit: Before using the sample, 2 weeks after using it, and 4 weeks after using it, the hair loss was counted by combing the hair 60 times, and the hair loss situation was collected and recorded. The test results are shown in Tables 14-15.

[0231] Table 14 Hair loss count (n=10)

[0232] Test time period Example 1 Comparative Example 1 Comparative Example 5 Week 0 average (root) 40 47 46 Average value of the second week (root) 23 33 35 Average value of the 4th week (root) 20 30 30

[0233] Table 15 The mean change rate of hair loss count relative to the initial value (n = 10)

[0234]

[0235]

[0236] From the above test results, it can be seen that Example 1 has a better anti-hair loss effect. Compared with Comparative Example 1, Example 1 adds 0.3% more guar hydroxypropyl trimethyl ammonium chloride, which shows that guar hydroxypropyl trimethyl ammonium chloride and Platycladus orientalis extract work together to produce a better synergistic anti-hair loss effect. Compared with Comparative Example 5, Example 1 uses a different type of Platycladus orientalis extract, which further shows that the Platycladus orientalis leaf extract in Example 1 is extracted using a special process, which can produce a flocculation effect with guar hydroxypropyl trimethyl ammonium chloride, promote better adsorption of the active ingredients on the hair and scalp, and thus produce a better anti-hair loss effect.

[0237] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. Anti-hair loss and oil control shampoo, characterized in that: It includes the following components by weight: 11-40 parts of surfactant, 2-20 parts of Platycladus orientalis extract, 0.1-0.8 parts of cationic conditioning agent, 0.05-0.2 parts of chelating agent, 0.3-1.3 parts of rheology modifier and 50-75 parts of water; The Platycladus orientalis extract comprises isoquercetin, afusadrin, aconitum biflavonoids, pine lactone and dextrorotatory quinic acid in a mass ratio of 1:(2-2.7):(3.5-5):(2-2.6):(650-890).

2. The anti-hair loss and oil control shampoo according to claim 1, characterized in that: In the Platycladus orientalis extract, the percentages of isoquercetin, afudamidin and aconitum biflavonoids in the total flavonoids are 0.30% to 1.00%, 0.60% to 1.90% and 3.50% to 3.90% respectively.

3. The anti-hair loss and oil control shampoo according to claim 1, characterized in that: The Platycladus orientalis extract also includes at least one of propylene glycol and butylene glycol.

4. The anti-hair loss and oil control shampoo according to claim 1, characterized in that: The Platycladus orientalis extract also includes PEG-40 hydrogenated castor oil and / or disodium EDTA; Preferably, in the Platycladus orientalis extract, the mass fraction of the PEG-40 hydrogenated castor oil is 0.2% to 0.6%, and the mass fraction of the disodium EDTA is 0.1% to 0.2%.

5. The anti-hair loss and oil control shampoo according to claim 1, characterized in that: The preparation of the Platycladus orientalis extract comprises: (a) using ethanol aqueous solution as the extraction solvent, with a solid-liquid ratio of 1:10 to 1:30, and extracting Platycladus orientalis leaves at 25 to 85°C for 1 to 3 hours; (b) adjusting the pH of the extract obtained by the extraction to 8.3-9.5, stirring the extract, filtering the extract, and then adjusting the pH to 7.0±0.

5.

6. The anti-hair loss and oil control shampoo according to claim 5, characterized in that: The preparation of the Platycladus orientalis extract further comprises: concentrating the material whose pH is adjusted to 7.0±0.5, and re-dissolving it with a propylene glycol aqueous solution or a butylene glycol aqueous solution; Preferably, PEG-40 hydrogenated castor oil and / or disodium EDTA are added to the re-dissolved material.

7. The anti-hair loss and oil control shampoo according to claim 1, characterized in that: The cationic conditioning agent includes at least one of guar hydroxypropyltrimonium chloride, polyquaternium-10, and polyquaternium-39.

8. The anti-hair loss and oil control shampoo according to claim 1, characterized in that: The mass ratio of the Platycladus orientalis extract to the cationic conditioning agent is (20-35):1; Preferably, the mass ratio of the Platycladus orientalis extract to the cationic conditioning agent is (30-35):

1.

9. The anti-hair loss and oil control shampoo according to claim 1, characterized in that: The anti-hair loss and oil control shampoo further comprises a pH regulator and / or a preservative; Preferably, the anti-hair loss and oil control shampoo further comprises the following components in parts by weight: 0.01 to 0.1 parts of a pH adjuster and 0.1 to 1 parts of a preservative.

10. The method for preparing the anti-hair loss and oil control shampoo according to any one of claims 1 to 9, characterized in that: The method comprises the following steps: mixing the components in proportion; Preferably, the method comprises the following steps: (A) mixing water, a chelating agent and a cationic conditioning agent in proportion and dissolving them, then adding a surfactant, heating to 80-85° C. and stirring until dissolved; (B) Cooling the material obtained in step (A) to below 45°C, adding the remaining materials and stirring evenly.

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