Application of dendrobium stem extract and sparassis crispa extract in preparation of cosmetics / medicines
Through the combination of Dendrobium stem extract, hydrangea extract and sodium hyaluronate, combined with extraction and treatment technology, the skin sensitivity and pore blockage caused by existing oil-controlled skin care products are solved, achieving significant oil-controlled effect and skin comfort sex.
Patent Information
- Application Number
- CN202411536290.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-31
- Publication Date
- 2025-01-10
- Estimated Expiration
- 2044-10-31
AI Technical Summary
Common ingredients of existing oil-controlled skin care products such as salicylic acid may cause skin sensitivity, oil-absorbing powder can easily lead to pore blockage, and there are many types of raw materials and limited oil control ability, making it difficult to effectively control sebaceous gland secretion and reduce skin oil output.
The composition of Dendrobium stem extract and hydrangea extract is combined with sodium hyaluronate, and mixed and extracted and filtered by water as the extraction solvent. The composition formed has good oil control effect and is homogenized, microwaved, and ultrasound. and micro-pressure treatment improve oil control effect.
It significantly improves the oil control effect, can effectively reduce oil synthesis, relieve skin oil problems, and the composition is gentle and non-irritating to the skin, and is suitable for cosmetics and pharmaceutical fields.
Smart Images

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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of skin care products, and in particular to application of a dendrobium stem extract and a hydrangea extract in preparing cosmetics / medicines. Background Art
[0002] Oily skin is mainly caused by the vigorous secretion of sebaceous glands, which makes the skin greasy and difficult to clean. It is also easy to cause acne, inflammation, desquamation, etc. due to the greasiness. Therefore, controlling the secretion of sebaceous glands and reducing oil production is the key to keeping this type of skin healthy and beautiful. In terms of market share, there is also a huge space in the oil control market.
[0003] The causes of oily skin are related to the internal environment of the endocrine, nervous and immune systems, and are also affected by the external environment, diet and other factors. The main ones are: 1. Age: Newborns have active sebaceous glands due to the influence of androgens in their mothers. After puberty, the gonads and adrenal glands produce more androgens, which enlarges the sebaceous glands and increases sebum. 2. Gender: After males enter puberty, the testicles begin to secrete androgens to promote the development of reproductive organs, the appearance of secondary sexual characteristics and sexual desire. At this time, the face is oily, the pores are large, the sebaceous glands secrete vigorously and the face is oily. The androgen in women is mainly secreted by the ovaries and adrenal glands, which can maintain normal reproductive function in women and maintain the normal development of female pubic hair, armpit hair, muscles and the whole body. If the female body secretes too much androgen, because androgen can inhibit the secretion of gonadotropin-releasing hormone by the hypothalamus and has the effect of counteracting estrogen, it will lead to increased oiliness of the female skin; ③ Endocrine: Androgen and adrenal cortex hormone in the human body can make the sebaceous glands hypertrophy and enhance the secretion function; ④ Greasy food, spicy food, high-sugar food, etc., make the spleen and stomach generate heat, which will lead to endogenous dampness and heat in the body in the long run, increasing sebum secretion; ⑤ Emotion: Human emotions can stimulate the parasympathetic nerves and endocrine system, strengthen the secretion of the endocrine system through feedback, increase androgen secretion, anxiety, staying up late can aggravate the oily state of the face, etc. All of the above factors can lead to oily face.
[0004] Due to the influence of people's living and working habits and the environment, the problem of oily skin is becoming more and more common. There is a great demand for the research and development of oil control products. However, the commonly used oil control ingredients such as salicylic acid often cause skin sensitivity to worsen during use. Oil control through oil-absorbing powders can easily lead to clogged pores. Plant extracts are used in oil control products, but there are usually many types of raw materials and their oil control capabilities are limited. Summary of the invention
[0005] One object of the present invention is to provide a use of a composition containing a Dendrobium stem extract and a Hydrangea sphaerocephala extract in the preparation of cosmetics / pharmaceuticals with oil-control effects.
[0006] In a specific embodiment of the present invention, the composition comprises 1 to 5 parts of Dendrobium stem extract and 1 to 5 parts of Hydrangea extract in parts by weight.
[0007] In a specific embodiment of the present invention, the composition comprises 3.5-4.5 parts of Dendrobium stem extract and 3-4 parts of Hydrangea extract in parts by weight.
[0008] In a specific embodiment of the present invention, the molecular weight of the dendrobium polysaccharide in the dendrobium stem extract is 10w-50wDa.
[0009] In a specific embodiment of the present invention, the composition further comprises sodium hyaluronate.
[0010] In a specific embodiment of the present invention, the amount of sodium hyaluronate is 0.05% to 0.5% by mass relative to the composition.
[0011] In a specific embodiment of the present invention, the amount of sodium hyaluronate is 0.1% to 0.2% by mass relative to the composition.
[0012] In a specific embodiment of the present invention, the mass ratio of the dendrobium polysaccharide in the dendrobium stem extract to the sodium hyaluronate is (1-6):1.
[0013] In a specific embodiment of the present invention, the preparation method of the composition comprises:
[0014] The stems of Dendrobium officinale and Hydrangea macrophylla are mixed and extracted with water as the extraction solvent at a solid-liquid ratio of 1:(10-80), and the extract is decolorized, deodorized and filtered.
[0015] In a specific embodiment of the present invention, the preparation method of the composition comprises:
[0016] (a) extracting, decolorizing, deodorizing, and filtering the stems of Dendrobium officinale using water as an extraction solvent at a solid-liquid ratio of 1:(10-80) to obtain a Dendrobium officinale polysaccharide extract;
[0017] (b) The polysaccharide extract of Dendrobium officinale and water are used to extract the hydrangea at a solid-liquid ratio of 1:(10-100), and then the extract is decolorized, deodorized and filtered.
[0018] In a specific embodiment of the present invention, in step (a), the filtrate obtained by filtration is separated by membrane separation, and the filtrate with a molecular weight between 10w and 50wDa is collected to obtain the Dendrobium polysaccharide extract.
[0019] In a specific embodiment of the present invention, the preparation method of the composition comprises:
[0020] The dendrobium stem and hydrangea sphaerocephala are extracted respectively with water as the extraction solvent and the solid-liquid ratio being 1:(10-100), and the extract is decolorized, deodorized and filtered; then the dendrobium stem extract and the hydrangea sphaerocephala extract are mixed and compounded.
[0021] In a specific embodiment of the present invention, the preparation method of the composition comprises:
[0022] (a1) extracting, decolorizing, deodorizing, and filtering the stems of Dendrobium officinale using water as an extraction solvent at a solid-liquid ratio of 1:(10-80), separating the extract using a membrane separation method, and collecting the stem extract of Dendrobium officinale with a molecular weight between 10w and 50wDa;
[0023] (b1) extracting the hydrangea with water at a solid-liquid ratio of 1:(10-80), and then decolorizing, deodorizing, and filtering the extract to obtain a hydrangea extract;
[0024] (c1) mixing the Dendrobium stem extract and the Hydrangea macrophylla extract.
[0025] In a specific embodiment of the present invention, the extraction temperature is 40 to 90° C.; the extraction time is 1 to 4 hours.
[0026] In a specific embodiment of the present invention, the decolorization and deodorization comprises: adding activated carbon or hydrogen peroxide to the extract for treatment, and collecting the filtrate.
[0027] In a specific embodiment of the present invention, before the extraction, the hydrangea is subjected to high temperature micro-pressure or water vapor treatment.
[0028] In a specific embodiment of the present invention, the preparation method of the composition further comprises: mixing the mixture of the Dendrobium stem extract and the Hydrangea extract with sodium hyaluronate in proportion, and subjecting the mixture to homogenization, microwave, ultrasound and / or micro-pressure treatment.
[0029] In a specific embodiment of the present invention, the Dendrobium stem extract and sodium hyaluronate are mixed in proportion, homogenized, microwaved, ultrasonically and / or micro-pressured, and then mixed with the Hydrangea extract.
[0030] In a specific embodiment of the present invention, the homogenization conditions include: a rotation speed of 2000 to 5000 rpm and a homogenization time of 5 to 30 minutes.
[0031] In a specific embodiment of the present invention, the micro-pressure conditions include: a temperature of 110 to 121° C., a gauge pressure of 0.05 to 0.13 MPa, and a micro-pressure time of 5 to 20 min.
[0032] In a specific embodiment of the present invention, the microwave conditions include: microwave power of 200-800w, and microwave time of 5-20min.
[0033] In a specific embodiment of the present invention, the ultrasonic conditions include: ultrasonic power of 50-400W, ultrasonic temperature of 30-60°C, and ultrasonic time of 5-20min.
[0034] Compared with the prior art, the present invention has the following beneficial effects:
[0035] (1) The composition containing the Dendrobium stem extract and the Hydrangea extract of the present invention has good oil control effect;
[0036] (2) The composition formed by the Dendrobium stem extract and the Hydrangea extract, as well as the composition formed by the Dendrobium stem extract, the Hydrangea extract and sodium hyaluronate, have a synergistic effect, and the oil control effect of the obtained composition is significantly improved; in particular, the ratio of the various components in the composition, especially the Dendrobium stem (extract) and the Hydrangea (extract) is maintained within the scope of protection claimed by the present invention, and the oil control effect of the composition is significantly improved. DETAILED DESCRIPTION
[0037] 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.
[0038] In a specific embodiment of the present invention, there is provided a use of a composition containing a Dendrobium stem extract and a Hydrangea sphaerocephala extract in the preparation of cosmetics / pharmaceuticals with oil-control effects.
[0039] Dendrobium nobile Lindl. can nourish yin and eliminate heat. Modern pharmacology shows that Dendrobium nobile Lindl. contains a variety of compounds such as alkaloids, polysaccharides, sesquiterpenes, flavonoids, etc., which can enhance immunity, relieve diabetes and its complications, anti-oxidation, anti-fatigue, and delay aging.
[0040] Sparassis crispa is rich in β-glucan, the most abundant in mushrooms. In addition, it also contains a variety of active ingredients such as protein, amino acids, vitamins, etc. Studies have shown that Sparassis crispa has a variety of functions such as anti-oxidation, inhibiting the release of inflammatory factors, and regulating the balance of helper T cells 1 and 2 (Th1 / Th2).
[0041] The applicant has found that a composition containing a Dendrobium stem extract and a Hydrangea macrophylla extract can be used as an oil-control composition, which has a simple type of raw materials, can reduce the synthesis of oil, and effectively alleviate the problem of oily skin.
[0042] The composition containing the Dendrobium stem extract and the Hydrangea extract of the present invention can be used in the preparation of cosmetics or medicines; wherein the cosmetics can be common types in the cosmetics field, for example, lotions, emulsions, creams, masks, sunscreens, makeup products, etc., and can also be shampoo products, bath products, etc., which may not be specifically limited. The type of medicine may also not be specifically limited.
[0043] In a specific embodiment of the present invention, when preparing cosmetics or medicines, the amount of the composition is in the range of 2wt%-50wt%; preferably, the range is 2wt%-20wt%; and more preferably, the range is 2.5wt%-10wt%.
[0044] In a specific embodiment of the present invention, the composition comprises 1 to 5 parts of Dendrobium stem extract and 1 to 5 parts of Hydrangea extract in parts by weight.
[0045] For example, in different embodiments, the composition may include 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5 or 5 parts of Dendrobium stem extract, and 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5 or 5 parts of Hydrangea extract, by weight. The amount of Dendrobium stem extract or Hydrangea extract may also be between any two of the above values.
[0046] In a specific embodiment of the present invention, the composition comprises 3.5-4.5 parts of Dendrobium stem extract and 3-4 parts of Hydrangea extract in parts by weight.
[0047] It should be noted that, in the composition of the present invention, the dosage of the Dendrobium stem extract and the Hydrangea spp. extract is calculated based on the dosage of the raw materials Dendrobium stem and Hydrangea spp., respectively.
[0048] In a specific embodiment of the present invention, the Dendrobium stem extract is a water extract of the Dendrobium stem, and the Hydrangea extract is a water extract of Hydrangea.
[0049] In a specific embodiment of the present invention, the molecular weight of the polysaccharide in the stem extract of Dendrobium officinale is 10w-50wDa. If the molecular weight of the polysaccharide in the stem extract of Dendrobium officinale is kept within the above range, the oil control effect of the obtained composition can be further improved.
[0050] For example, in different embodiments, the molecular weight of Dendrobium polysaccharide can be exemplified as 10w, 12w, 16w, 20w, 23w, 25w, 28w, 30w, 33w, 35w, 37w, 40w, 42w, 46w, 50wDa or a range between any two values, etc.
[0051] In a specific embodiment of the present invention, the dendrobium polysaccharide with a molecular weight of 10w-50wDa includes at least mannose, galacturonic acid, glucose, galactose, xylose, arabinose and fucose. Further, the dendrobium polysaccharide includes at least 77-78 parts of mannose, 0.05-0.1 parts of galacturonic acid, 18-25 parts of glucose, 0.5-1 parts of galactose, 0.2-0.6 parts of xylose, 0.05-0.1 parts of arabinose and 0.05-0.1 parts of fucose by weight.
[0052] Monosaccharide molecules are the basic components of polysaccharides, which are formed through condensation and dehydration. In the connection between monosaccharide composition and activity, studies have found that the functional activity of polysaccharides has direct and indirect connections with their monosaccharide composition. For example, the immunostimulatory activity and antioxidant activity of polysaccharides are affected by the relative content of monosaccharides. According to analysis, the monosaccharide composition of the dendrobium polysaccharide in the dendrobium extract of the present invention is mainly mannose and glucose, and also contains galacturonic acid, galactose, xylose, arabinose and fucose.
[0053] In a specific embodiment of the present invention, the composition further includes sodium hyaluronate. When the composition includes a Dendrobium stem extract, a Hydrangea extract and sodium hyaluronate, the oil control effect of the composition is significantly further improved. Among them, sodium hyaluronate can be prepared by itself, or a commercial product can be used, such as a commercial product of Shandong Galaxy Biotechnology Co., Ltd.
[0054] In a specific embodiment of the present invention, the amount of sodium hyaluronate is 0.05wt% to 0.5wt% based on the mass percentage of the composition.
[0055] In a specific embodiment of the present invention, the amount of sodium hyaluronate can be 0.05wt%, 0.08wt%, 0.1wt%, 0.12wt%, 0.15wt%, 0.18wt%, 0.2wt%, 0.23wt%, 0.25wt%, 0.27wt%, 0.3wt%, 0.34wt%, 0.37wt%, 0.4wt%, 0.42wt% / 0.45wt%, 0.48wt% or 0.5wt%, based on the mass percentage relative to the composition, or it can be an amount between any two of the above values.
[0056] In a specific embodiment of the present invention, the amount of sodium hyaluronate is 0.1 wt % to 0.2 wt % based on the mass percentage of the composition.
[0057] In a specific embodiment of the present invention, the molecular weight of sodium hyaluronate is 1000Da to 200wDa.
[0058] For example, in different embodiments, the molecular weight of the sodium hyaluronate can be exemplified as 1000, 5000, 8000, 1w, 3w, 5w, 8w, 10w, 15w, 20w, 40w, 50w, 70w, 100w, 130w, 170w or 200wDa or a range between any two of the above values, etc.
[0059] In a specific embodiment of the present invention, in the composition, the mass ratio of the dendrobium polysaccharide in the dendrobium stem extract to the sodium hyaluronate is (1-6):1.
[0060] For example, in different embodiments, the mass ratio of the dendrobium polysaccharide in the dendrobium stem extract to the sodium hyaluronate can be exemplified as 1:1, 1.3:1, 1.8:1, 2:1, 2.5:1, 3:1, 3.3:1, 3.5:1, 4:1, 4.2:1, 4.5:1, 4.8:1, 5:1, 5.5:1, 5.8:1 or 6:1, or it can be a ratio between any two of the above ratios.
[0061] In a specific embodiment of the present invention, the composition further comprises an additive. Further, the additive comprises a polyol and / or a preservative. The polyol comprises at least one of glycerol, propylene glycol, butylene glycol, pentylene glycol, hexylene glycol or other polyols commonly used in skin care products; the preservative comprises at least one of phenoxyethanol, ethylhexylglycerin or other preservatives commonly used in skin care products.
[0062] For example, in different embodiments, a combination of glycerin, pentylene glycol and hexylene glycol may be used, or a combination of glycerin, phenoxyethanol and ethylhexylglycerin may be used.
[0063] In a specific embodiment of the present invention, the amount of glycerol is 0% to 50wt% in terms of weight percentage relative to the composition; preferably, the amount of glycerol is 10wt% to 25wt%; in the composition, the amounts of pentanediol, hexylene glycol, phenoxyethanol and ethylhexylglycerin are 1wt% to 3wt%, 0.5wt% to 2wt%, 0.45wt% to 0.63wt% and 0.05wt% to 0.07wt%, respectively.
[0064] For example, in different embodiments, the content of glycerol in the composition can be 0wt%, 1wt%, 5wt%, 10wt%, 12wt%, 18wt%, 20wt%, 25wt%, 30wt%, 35wt%, 40wt%, 42wt%, 45wt%, 48wt% or 50wt%, etc.; the amount of other additives in the composition can be adjusted according to actual conditions.
[0065] In a specific embodiment of the present invention, the dendrobium includes Dendrobium officinale Kimura & Migo.
[0066] In a specific embodiment of the present invention, the preparation method of the composition comprises the following steps: mixing and compounding the Dendrobium stem extract and the Hydrangea sphaerocephala extract.
[0067] In a specific embodiment of the present invention, the preparation method comprises the following steps: using water as an extraction solvent, the solid-liquid ratio is 1:(10-80) (m / m) to mix and extract the Dendrobium stems and Hydrangea, and decolorizing, deodorizing and filtering the extract.
[0068] In the above embodiment, water is used as the extraction solvent to extract the mixed Dendrobium stem and Hydrangea. In different embodiments, the solid-liquid ratio can be exemplarily 1:10 (m / m), 1:12 (m / m), 1:15 (m / m), 1:20 (m / m), 1:30 (m / m), 1:40 (m / m), 1:45 (m / m), 1:48 (m / m), 1:50 (m / m), 1:60 (m / m), 1:70 (m / m), 1:73 (m / m), 1:77 (m / m) or 1:80 (m / m), etc., or it can be a ratio between any two of the above ratios.
[0069] In a specific embodiment of the present invention, the preparation method comprises the following steps: using water as an extraction solvent and a solid-liquid ratio of 1:(10-100) (m / m) to extract Dendrobium stems and Hydrangea spp. respectively, decolorizing, deodorizing and filtering the extract; and then mixing and compounding the Dendrobium stem extract and the Hydrangea spp. extract.
[0070] In the above embodiment, water is used as the extraction solvent to extract the stem of Dendrobium and the hydrangea respectively, obtain the corresponding stem extract of Dendrobium and the hydrangea extract, and then mix and compound. For example, in different embodiments, the solid-liquid ratio can be exemplarily 1:10 (m / m), 1:12 (m / m), 1:15 (m / m), 1:20 (m / m), 1:30 (m / m), 1:40 (m / m), 1:45 (m / m), 1:50 (m / m), 1:54 (m / m), 1:58 (m / m), 1:60 (m / m), 1:65 (m / m), 1:70 (m / m), 1:80 (m / m), 1:90 (m / m), 1:95 (m / m), 1:98 (m / m) or 1:100 (m / m), etc.
[0071] In a specific embodiment of the present invention, the preparation method comprises the following steps:
[0072] (a) extracting, decolorizing, deodorizing, and filtering the stems of Dendrobium officinale using water as an extraction solvent at a solid-liquid ratio of 1:(10-80) (m / m) to obtain a Dendrobium officinale polysaccharide extract;
[0073] (b) extracting the hydrangea with the dendrobium polysaccharide extract and water at a solid-liquid ratio of 1:(10-100) (m / m), and then decolorizing, deodorizing, and filtering the extract.
[0074] In the above embodiment, water is used as the extraction solvent, the stem of Dendrobium is first extracted, the stem extract of Dendrobium is subjected to membrane separation, and the Dendrobium polysaccharide extract with a molecular weight between 10w and 50wDa is collected; then the Dendrobium polysaccharide extract and water are used as the extraction solvent to extract the hydrangea. For example, in different embodiments, in step (a), the solid-liquid ratio can be exemplarily 1:10 (m / m), 1:12 (m / m), 1:15 (m / m), 1:20 (m / m), 1:30 (m / m), 1:40 (m / m), 1:45 (m / m), 1:48 (m / m), 1:50 (m / m), 1:60 (m / m), 1:70 (m / m), 1:73 (m / m), 1:77 (m / m) or 1: 80 (m / m), etc.; in step (b), the material-liquid ratio can be exemplarily 1:10 (m / m), 1:15 (m / m), 1:20 (m / m), 1:30 (m / m), 1:40 (m / m), 1:50 (m / m), 1:60 (m / m), 1:70 (m / m), 1:80 (m / m), 1:90 (m / m), 1:95 (m / m), 1:98 (m / m) or 1:100 (m / m), etc.
[0075] It should be noted that in step (b), the dendrobium polysaccharide extract and water are used as extraction solvents to extract the hydrangea, and the solid-liquid ratio refers to the mass and ratio of the hydrangea to the dendrobium polysaccharide extract and water.
[0076] In a specific embodiment of the present invention, in step (a), the filtrate obtained by filtration is separated by membrane separation, and the filtrate with a molecular weight between 10w and 50wDa is collected to obtain the above-mentioned Dendrobium polysaccharide extract.
[0077] In another specific embodiment of the present invention, the preparation method comprises the following steps:
[0078] (a1) extracting, decolorizing, deodorizing, and filtering the stems of Dendrobium officinale using water as an extraction solvent at a solid-liquid ratio of 1:(10-80) (m / m), separating the extract using a membrane separation method, and collecting a Dendrobium officinale polysaccharide extract having a molecular weight of 10w-50wDa;
[0079] (b1) extracting the hydrangea with water at a solid-liquid ratio of 1:(10-80) (m / m), and then decolorizing, deodorizing, and filtering the extract to obtain a hydrangea extract;
[0080] (c1) mixing the Dendrobium polysaccharide extract and the Hydrangea macrophylla extract.
[0081] In the above embodiment, water is used as an extraction solvent, the stem of Dendrobium is first extracted, the stem extract of Dendrobium is subjected to membrane separation, and a Dendrobium polysaccharide extract having a molecular weight between 10w and 50wDa is collected; then, the hydrangea is extracted with water as an extraction solvent to obtain a hydrangea extract; and the Dendrobium polysaccharide extract is compounded with the hydrangea extract. For example, in different embodiments, in step (a1) and step (b1), the solid-liquid ratio can be exemplarily 1:10 (m / m), 1:12 (m / m), 1:15 (m / m), 1:20 (m / m), 1:30 (m / m), 1:40 (m / m), 1:45 (m / m), 1:48 (m / m), 1:50 (m / m), 1:60 (m / m), 1:70 (m / m), 1:73 (m / m), 1:77 (m / m) or 1:80 (m / m), etc.
[0082] In a specific embodiment of the present invention, the extraction temperature is 40 to 90° C.; the extraction time is 1 to 4 hours.
[0083] For example, in different embodiments, the extraction temperature can be exemplified as 40°C, 45°C, 50°C, 55°C, 60°C, 65°C, 70°C, 75°C, 80°C, 85°C, 90°C, etc.; the extraction time can be exemplified as 1h, 1.2h, 1.5h, 2h, 2.5h, 3h, 3.5h, 3.8h or 4h, etc.
[0084] In a specific embodiment of the present invention, before the extraction, the extraction solvent and the Dendrobium stem, or the mixture of the extraction solvent, the Dendrobium stem and Hydrangea spp., are stirred at room temperature for 20 to 60 minutes.
[0085] For example, in different embodiments, the stirring time at room temperature can be 20 min, 22 min, 25 min, 30 min, 35 min, 38 min, 40 min, 42 min, 45 min, 50 min, 55 min, 58 min or 60 min, etc.
[0086] In a specific embodiment of the present invention, the decolorization and deodorization comprises: adding activated carbon or hydrogen peroxide to the extract for treatment, and collecting the filtrate. Further, the amount of activated carbon added is 0.1wt% to 2wt% of the extract; the amount of hydrogen peroxide added is 0.01wt% to 1wt% of the extract.
[0087] In a specific embodiment of the present invention, before extraction, the hydrangea is subjected to high temperature micro-pressure or water vapor treatment. Further, the high temperature micro-pressure treatment includes: a temperature of 110-121°C, a gauge pressure of 0.05-0.13 MPa, and a micro-pressure time of 5-20 min; the water vapor treatment includes: steaming at 90-100°C for 5-20 min.
[0088] In a specific embodiment of the present invention, before the extraction, the stem of Dendrobium officinale is crushed and sieved to obtain the sieved material.
[0089] In a specific embodiment of the present invention, the filtration treatment includes: coarse filtration and fine filtration. Further, the coarse filtration includes cardboard filtration; the fine filtration includes cardboard filtration and diatomaceous earth filtration.
[0090] In actual operation, the paperboard filtration in the coarse filtration may be F100 paperboard filtration; after the coarse filtration, the coarse filtrate is cooled to below 35° C. and then fine filtration is performed. In the fine filtration, the paperboard filtration may be H70 paperboard filtration.
[0091] In a specific embodiment of the present invention, the preparation method of the composition further includes: mixing the mixture of the Dendrobium stem extract and the Hydrangea extract with sodium hyaluronate in proportion, and subjecting the mixture to homogenization, microwave, ultrasound and / or micro-pressure treatment. In actual operation, sodium hyaluronate is compounded into the refined filtrate obtained by the filtration treatment; and polyols such as glycerol are compounded into the refined filtrate.
[0092] In a specific embodiment of the present invention, the preparation method of the composition further comprises: mixing the Dendrobium stem extract and sodium hyaluronate in proportion, subjecting to homogenization, microwave, ultrasound and / or micro-pressure treatment, and then mixing with the Hydrangea extract. The Dendrobium stem extract may be a Dendrobium stem extract that has not been subjected to membrane separation, or a Dendrobium polysaccharide extract that has been subjected to membrane separation.
[0093] In actual operation, sodium hyaluronate and glycerin can be compounded with the refined filtrate, and then subjected to subsequent homogenization, microwave, ultrasound and / or micro-pressure treatment; or after adding the hydrangea extract and mixing, glycerin can be added for compounding.
[0094] In a specific embodiment of the present invention, the homogenization conditions include: a rotation speed of 2000-5000rpm, and a homogenization time of 5-30min; the micro-pressure conditions include: a temperature of 110-121°C, a gauge pressure of 0.05-0.13MPa, and a micro-pressure time of 5-20min; the microwave conditions include: a microwave power of 200-800W, and a microwave time of 5-20min; the ultrasonic conditions include: an ultrasonic power of 50-400W, an ultrasonic temperature of 30-60°C, and an ultrasonic time of 5-20min.
[0095] For example, in different embodiments, in the homogenization, the rotation speed can be exemplarily 2000rpm, 2200rpm, 2500rpm, 3000rpm, 3500rpm, 4000rpm, 4500rpm, 47rpm or 5000rpm, etc., and the homogenization time can be exemplarily 5min, 8min, 10min, 12min, 15min, 18min, 20min, 25min, 28min, 30min, etc.; in the micro-pressure, the temperature can be exemplarily 110°C, 112°C, 115°C, 118°C, 120°C, 121°C, etc., the gauge pressure can be exemplarily 0.05MPa, 0.06MPa, 0.08MPa, 0.1MPa, 0.11MPa, 0.12MPa, 0.13MPa, etc., and the micro-pressure time can be exemplarily 5m in, 8min, 10min, 12min, 15min, 18min, 20min, etc.; in the microwave, the microwave power can be exemplarily 200W, 250W, 300W, 400W, 500W, 600W, 700W, 750W or 800W, etc., and the microwave time can be exemplarily 5min, 8min, 10min, 12min, 15min, 18min, 20min, etc.; in the ultrasound, the ultrasonic power can be exemplarily 50W, 100W, 150W, 200W, 250W, 300W, 350W, 400W, etc., the ultrasonic temperature can be exemplarily 30°C, 40°C, 50°C, 60°C, etc., and the ultrasonic time can be exemplarily 5min, 8min, 10min, 12min, 15min, 18min, 20min, etc.
[0096] In a specific embodiment of the present invention, it also includes: adding any one or more of propylene glycol, butylene glycol, pentylene glycol, hexylene glycol or other polyols commonly used in cosmetics, and / or any one or more of phenoxyethanol, ethylhexylglycerin or other preservatives commonly used in cosmetics to the composite liquid after homogenization, microwave, ultrasound and / or micro-pressure treatment according to actual needs, then stirring and sterilizing at 80-100° C. for 30-60 minutes, and cooling and filling.
[0097] The following embodiments and experimental examples are used to illustrate the technical solutions of the present invention.
[0098] Embodiments 1 to 4
[0099] The preparation method of the composition comprises:
[0100] (1) Raw material pretreatment: Weigh the hydrangea and treat it with high temperature and micro-pressure (110-121°C, 5-20 min), and crush the stems of Dendrobium officinale through an 80-mesh sieve;
[0101] (2) Extraction: Weigh the stems of Dendrobium officinale and Hydrangea spp. according to the proportion, add pure water at a solid-liquid ratio of 1:10 to 1:80 (m / m), stir at room temperature for 20 to 60 minutes, and then extract at 40 to 90° C. for 1 to 4 hours; after the extraction, add 0.1% to 0.2% activated carbon for decolorization and deodorization, and then filter with gauze to collect the filtrate;
[0102] (3) Filtration: The filtrate obtained in step (2) is filtered through F100 paperboard to collect the coarse filtrate; the coarse filtrate is then cooled to below 35° C., filtered through H70 paperboard and diatomaceous earth to collect the fine filtrate;
[0103] (4) Compounding: Compounding a certain amount of glycerol with the obtained refined filtrate to obtain a compounded liquid;
[0104] (5) Sterilization: Add 1,2-pentanediol and 1,2-hexanediol, or phenoxyethanol and ethylhexylglycerin to the compound solution of step (4), sterilize by stirring at 80-100° C. (e.g., 98-100° C.) for 30-60 min (e.g., 40 min), and fill after cooling.
[0105] The parameter conditions of different steps in Examples 1 to 4 are shown in Table 1.
[0106] Table 1 Process parameters of Examples 1 to 4
[0107] Example 1 Example 2 Example 3 Example 4 High temperature micro pressure treatment 120℃、5min 110℃, 20min 110℃, 5min 120℃、5min Dendrobium stem: Hydrangea 1:1 4:3.5 1:5 5:1 Material-liquid ratio (m / m) 1:10 1:40 1:80 1:80 Stirring time at room temperature (min) 60 30 20 20 Extraction temperature (℃) 90 60 40 40 Extraction time (h) 1 2 4 2 Activated carbon addition amount (%) 0.1 0.5 0.3 0.3 glycerin(%) 10 30 23 23 1,2-Pentanediol(%) 3 1 / / 1,2-Hexanediol(%) 0.5 1.5 / / Phenoxyethanol(%) / / 0.63 0.63 Ethylhexylglycerin (%) / / 0.07 0.07
[0108] Note: The amount of glycerol in Table 1 refers to the mass fraction of the compound liquid, and the amount of 1,2-pentanediol, 1,2-hexanediol, phenoxyethanol and ethylhexylglycerin refers to the mass fraction of the final product.
[0109] Embodiments 5 to 7
[0110] The preparation method of the composition comprises:
[0111] (1) Raw material pretreatment: Weigh the hydrangea and treat it with high temperature and micro-pressure (110-121°C, 5-20 min), and crush the stems of Dendrobium officinale through an 80-mesh sieve;
[0112] (2) Extraction: Weigh the stem of Dendrobium officinale, add pure water at a solid-liquid ratio of 1:10 to 1:80 (m / m), stir at room temperature for 20 to 60 minutes, and then extract at 40 to 90° C. for 1 to 4 hours; after the extraction, add 0.1% to 2% activated carbon for decolorization and deodorization, and then filter with gauze to collect the filtrate;
[0113] (3) adding a certain amount of water (all of the filtrate is used, and the rest is supplemented with water) to the filtrate obtained in step (2), and adding the hydrangea to the hydrangea at a solid-liquid ratio of 1:10 to 1:100 (m / m), stirring at room temperature for 20 to 60 minutes, and then extracting at 40 to 90° C. for 1 to 4 hours; after the extraction is completed, adding 0.1% to 2% activated carbon for decolorization and deodorization, and then filtering with gauze to collect the filtrate;
[0114] (4) Filtration: The filtrate obtained in step (3) is filtered through F100 paperboard to collect the coarse filtrate; the coarse filtrate is then cooled to below 35° C., filtered through H70 paperboard + diatomaceous earth, and the fine filtrate is collected;
[0115] (5) Compounding: compounding a certain amount of glycerol into the refined filtrate obtained in step (4) to obtain a compounded liquid;
[0116] (6) Sterilization: Add 1,2-pentanediol and 1,2-hexanediol, or phenoxyethanol and ethylhexylglycerol to the compound solution of step (5), sterilize by stirring at 80-100° C. (e.g., 98-100° C.) for 30-60 min (e.g., 40 min), and fill after cooling.
[0117] The parameter conditions of different steps in Examples 5 to 7 are shown in Table 2.
[0118] Table 2 Process parameters of Examples 5 to 7
[0119] Example 5 Example 6 Example 7 High temperature micro pressure treatment 120℃、5min 110℃, 20min 110℃, 10min Dendrobium stem: Hydrangea 1:1 4:3.5 5:1 Material-liquid ratio (m / m) 1:10;1:100 1:40;1:60 1:80;1:10 Stirring time at room temperature (min) 60;60 30;30 20;20 Extraction temperature (℃) 90;90 60;60 40;40 Extraction time (h) 1;1 2;2 4;4 Activated carbon addition amount (%) 0.1;0.1 0.5;0.5 0.3;0.3 glycerin(%) 10 23 30 1,2-Pentanediol(%) 3 1 / 1,2-Hexanediol(%) 0.5 1.5 / Phenoxyethanol(%) / / 0.63 Ethylhexylglycerin (%) / / 0.07
[0120] Note: The amount of glycerol in Table 2 refers to the mass fraction of the compound liquid, and the amount of 1,2-pentanediol, 1,2-hexanediol, phenoxyethanol and ethylhexylglycerin refers to the mass fraction of the final product.
[0121] Embodiments 8 to 10
[0122] The preparation method of the composition comprises:
[0123] (1) Raw material pretreatment: Weigh the hydrangea and treat it with high temperature and micro-pressure (110-121°C, 5-20 min), and crush the stems of Dendrobium officinale and pass through an 80-day sieve;
[0124] (2) Extraction: Weigh the stem of Dendrobium officinale, add pure water at a solid-liquid ratio of 1:10 to 1:80 (m / m), stir at room temperature for 20 to 60 minutes, and then extract at 40 to 90° C. for 1 to 4 hours; after the extraction, add 0.1% to 2% activated carbon for decolorization and deodorization, and then fine filter to collect the filtrate;
[0125] (3) membrane separation: filtering the filtrate obtained in step (2) using 10wDa and 50wDa membranes to collect the Dendrobium polysaccharide extract with a molecular weight between 10w and 50wDa;
[0126] (4) Add a certain amount of water to the dendrobium polysaccharide extract in step (3) (all the dendrobium polysaccharide extract is used, and the rest is supplemented with water), and add the hydrangea to the extract at a solid-liquid ratio of 1:10 to 1:100 (m / m), stir at room temperature for 20 to 60 minutes, and then extract at 40 to 90° C. for 1 to 4 hours; add 0.1% to 2% activated carbon for decolorization and deodorization, and then filter with gauze to collect the filtrate;
[0127] (5) Filtration: The filtrate obtained in step (4) is filtered through F100 paperboard to collect the coarse filtrate; the coarse filtrate is then cooled to below 35° C., filtered through H70 paperboard + diatomaceous earth, and the fine filtrate is collected;
[0128] (6) Compounding: compounding a certain amount of glycerol into the refined filtrate obtained in step (5) to obtain a compounded solution;
[0129] (7) Sterilization: Add 1,2-pentanediol and 1,2-hexanediol, or phenoxyethanol and ethylhexylglycerol to the compound solution of step (6), and sterilize by stirring at 80 to 100° C. (e.g., 98 to 100° C.) for 30 to 60 min (e.g., 40 min), and then fill after cooling.
[0130] The parameter conditions of different steps in Examples 8 to 10 are shown in Table 3.
[0131] Table 3 Process parameters of Examples 8 to 10
[0132] Example 8 Example 9 Example 10 High temperature micro pressure treatment 120℃、5min 110℃, 20min 110℃, 5min Dendrobium stem: Hydrangea 1:1 4:3.5 1:5 Material-liquid ratio (m / m) 1:10;1:100 1:40;1:60 1:80;1:10 Stirring time at room temperature (min) 60;60 30;30 20;20 Extraction temperature (℃) 90;90 60;60 40;40 Extraction time (h) 1;1 2;2 4;4 Activated carbon addition amount (%) 0.1;0.1 0.5;0.5 0.3;0.3 glycerin(%) 10 30 23 1,2-Pentanediol(%) 3 1 / 1,2-Hexanediol(%) 0.5 1.5 / Phenoxyethanol(%) / / 0.63 Ethylhexylglycerin (%) / / 0.07
[0133] Note: The amount of glycerol in Table 3 refers to the mass fraction of the compound liquid, and the amount of 1,2-pentanediol, 1,2-hexanediol, phenoxyethanol and ethylhexylglycerin refers to the mass fraction of the final product.
[0134] Examples 11 to 14
[0135] The preparation method of the composition comprises:
[0136] (1) Raw material pretreatment: Weigh the hydrangea and treat it under high temperature and high pressure (110-121°C, 5-20 min), and crush the Dendrobium officinale through an 80-mesh sieve;
[0137] (2) Extraction: Weigh the stems of Dendrobium officinale and Hydrangea spp. according to the proportion, add pure water at a solid-liquid ratio of 1:10 to 1:80 (m / m), stir at room temperature for 20 to 60 minutes, and extract at 40 to 90° C. for 1 to 4 hours; after the extraction, add 0.1% to 2% activated carbon for decolorization and deodorization, and then filter with 200-mesh gauze to collect the filtrate;
[0138] (3) Filtration: The filtrate of step (2) is filtered through F100 paperboard to collect the coarse filtrate; the coarse filtrate is then cooled to below 35° C., filtered through H70 paperboard + diatomaceous earth, and the fine filtrate is collected;
[0139] (4) Compounding: compounding a certain amount of glycerol and 0.05% to 0.5% sodium hyaluronate into the refined filtrate obtained in step (3) to obtain a compound solution;
[0140] (5) Compound liquid treatment: the compound liquid of step (4) is placed in a homogenizer at a speed of 2000 to 5000 rpm (e.g., 2500 rpm) and homogenized for 5 to 30 min (e.g., 10 min);
[0141] (6) Sterilization: Add 1% to 3% 1,2-pentanediol and 0.5% to 1.5% 1,2-hexanediol, or 0.45% to 0.63% phenoxyethanol and 0.05% to 0.07% ethylhexylglycerol to the composite solution of step (4), sterilize with stirring at 98 to 100° C. (e.g. 98 to 100° C.) for 30 to 60 min (e.g. 40 min), and cool to room temperature for storage.
[0142] The parameter conditions of different steps in Examples 11 to 14 are shown in Table 4.
[0143] Table 4 Process parameters of Examples 11 to 14
[0144] Embodiment 11 Example 12 Example 13 Embodiment 14 High temperature micro pressure treatment 120℃、5min 110℃, 20min 110℃, 10min 110℃, 10min Dendrobium stem: Hydrangea 1:1 4:3.5 5:1 1:5 Material-liquid ratio (m / m) 1:10 1:40 1:80 1:80 Stirring time at room temperature (min) 60 30 20 20 Extraction temperature (℃) 90 60 40 40 Extraction time (h) 1 2 4 4 Activated carbon addition amount (%) 0.1 0.5 0.3 0.3 glycerin(%) 10 23 30 30 Sodium hyaluronate (%) 0.5 0.1 0.5 0.5 1,2-Pentanediol(%) 3 1 / / 1,2-Hexanediol(%) 0.5 1.5 / / Phenoxyethanol(%) / / 0.63 0.63 Ethylhexylglycerin (%) / / 0.07 0.07
[0145] Note: The amounts of glycerol and sodium hyaluronate in Table 4 refer to the mass fractions of the compound solution, and the amounts of 1,2-pentanediol, 1,2-hexanediol, phenoxyethanol and ethylhexylglycerin refer to the mass fractions of the final product.
[0146] Embodiments 15 to 18
[0147] The preparation method of the composition comprises:
[0148] (1) Raw material pretreatment: Weigh the hydrangea and treat it under high temperature and high pressure (110-121°C, 5-20 min). Crush the Dendrobium officinale and pass it through an 80-mesh sieve.
[0149] (2) Extraction: Weigh the stem of Dendrobium officinale, add pure water at a solid-liquid ratio of 1:10 to 1:80 (m / m), stir at room temperature for 20 to 60 min, and extract at 40 to 90° C. for 1 to 4 h; after the extraction, add 0.1% to 2% activated carbon for decolorization and deodorization, then filter with 200-mesh gauze to collect the filtrate.
[0150] (3) Membrane separation: The filtrate obtained in step (2) was filtered using 10w and 50w membranes to collect the Dendrobium polysaccharide extract with a molecular weight between 10wDa and 50wDa.
[0151] (4) Add a certain amount of water to the Dendrobium polysaccharide extract in step (3) (all the Dendrobium polysaccharide extract is used, and the rest is supplemented with water), and add it to the hydrangea at a solid-liquid ratio of 1:10 to 1:100, stir at room temperature for 20 to 60 minutes, and then extract at 40 to 90° C. for 1 to 4 hours; after the extraction is completed, add 0.1% to 2% activated carbon for decolorization and deodorization, filter through 200 mesh gauze, and collect the filtrate.
[0152] (5) Filtration: The filtrate obtained in step (4) is filtered through F100 paperboard to collect the coarse filtrate; the coarse filtrate is then cooled to below 35° C., filtered through H70 paperboard + red diatomaceous earth, and the fine filtrate is collected.
[0153] (6) Compounding: Compounding a certain amount of glycerol and 0.05% to 0.5% sodium hyaluronate into the refined filtrate of step (5) to obtain a compound solution.
[0154] (7) Treatment of the composite liquid: Place the composite liquid of step (6) in a homogenizer and homogenize at a speed of 2000 to 5000 rpm (e.g., 2500 rpm) for 5 to 30 min (e.g., 10 min).
[0155] (8) Sterilization: Add 1% to 3% 1,2-pentanediol and 0.5% to 1.5% 1,2-hexanediol, or 0.5% to 0.7% phenoxyethanol and 0.05% to 0.1% ethylhexylglycerol to the composite solution treated in step (7), sterilize with stirring at 80 to 100° C. (e.g., 98 to 100° C.) for 30 to 50 min (e.g., 40 min), and cool to room temperature for storage.
[0156] The parameter conditions of different steps in Examples 15 to 18 are shown in Table 5.
[0157] Table 5 Process parameters of Examples 15 to 18
[0158] Embodiment 15 Example 16 Embodiment 17 Embodiment 18 High temperature micro pressure treatment 120℃、5min 110℃, 20min 110℃, 10min 110℃, 10min Dendrobium stem: Hydrangea 1:1 4:3.5 5:1 1:5 Material-liquid ratio (m / m) 1:10;1:100 1:40;1:60 1:80;1:10 1:80;1:10 Stirring time at room temperature (min) 60;60 30;30 20;20 20;20 Extraction temperature (℃) 90;90 60;60 40;40 40;40 Extraction time (h) 1;1 2;2 4;4 4;4 Activated carbon addition amount (%) 0.1;0.1 0.5;0.5 0.3;0.3 0.3;0.3 glycerin(%) 10 23 30 30 Sodium hyaluronate (%) 0.5 0.1 0.5 0.5 1,2-Pentanediol(%) 3 1 / / 1,2-Hexanediol(%) 0.5 1.5 / / Phenoxyethanol(%) / / 0.63 0.63 Ethylhexylglycerin (%) / / 0.07 0.07
[0159] Note: The amounts of glycerol and sodium hyaluronate in Table 5 refer to the mass fractions of the compound solution, and the amounts of 1,2-pentanediol, 1,2-hexanediol, phenoxyethanol and ethylhexylglycerin refer to the mass fractions of the final product.
[0160] Embodiment 19
[0161] The preparation method of the composition comprises the following steps:
[0162] (1) Raw material pretreatment: Weigh the Hydrangea spp. and treat it with high temperature and micro-pressure (110°C, 20 min). Crush and sieve the stems of Dendrobium officinale. The mass ratio of the stems of Dendrobium officinale to Hydrangea spp. is 4:3.5.
[0163] (2) Extraction: Weigh the stem of Dendrobium officinale, add pure water at a solid-liquid ratio of 1:40 (m / m), stir at room temperature for 30 min, then extract at 60°C for 2 h, then add 0.5% activated carbon for decolorization and deodorization, then fine filter, and collect the filtrate.
[0164] (3) Membrane separation: The filtrate obtained in step (2) was filtered using 10wDa and 50wDa membranes to collect the Dendrobium polysaccharide extract with a molecular weight between 10w and 50wDa.
[0165] (4) Compounding the dendrobium polysaccharide extract in step (3) with sodium hyaluronate to obtain a compound solution; placing the compound solution in a homogenizer and homogenizing at a speed of 2000 to 5000 rpm (e.g., 2500 rpm) for 5 to 30 min (e.g., 10 min).
[0166] (5) Extraction of Hydrangea: Hydrangea was mixed with water at a solid-liquid ratio of 1:60 (m / m), stirred at room temperature for 30 min, and then extracted at 60°C for 2 h. After the extraction, 0.5% activated carbon was added for decolorization and deodorization, and then fine filtration was performed to collect the filtrate.
[0167] (6) Compounding: The compounded liquid after homogenization in step (4) is mixed with the filtrate obtained in step (5) to obtain a mixed liquid, and 23% glycerol (by mass fraction of the mixed liquid) is added.
[0168] (7) Sterilization: Add 1% 1,2-pentanediol and 1.5% 1,2-hexanediol (mass fraction of the final product) to the material obtained in step (6), sterilize by stirring at 80-100° C. (e.g. 98-100° C.) for 30-50 min (e.g. 40 min), and fill after cooling.
[0169] The amount of sodium hyaluronate used in step (4) is 0.15% of the sum of the mass of the Dendrobium polysaccharide extract in step (3), the hydrangea extract filtrate obtained in step (5) and the glycerol in step (6).
[0170] Embodiment 20
[0171] This example refers to the preparation method of the composition of Example 16, with the only difference being that step (3) is different.
[0172] Step (3) of this embodiment includes: filtering the filtrate obtained in step (2) using 1wDa and 10wDa membranes to collect the Dendrobium polysaccharide extract with a molecular weight between 1w and 10wDa.
[0173] Embodiment 21
[0174] This example refers to the preparation method of the composition of Example 16, with the only difference being that step (3) is different.
[0175] Step (3) of this embodiment includes: filtering the filtrate obtained in step (2) using 1000Da and 1wDa membranes to collect the Dendrobium polysaccharide extract with a molecular weight between 1000Da and 1wDa.
[0176] Embodiment 22
[0177] This example is based on the preparation method of the composition of Example 15, with the only difference being that in step (1), the hydrangea is not subjected to high temperature micro-pressure treatment.
[0178] Comparative Example 1
[0179] The composition was prepared by the same method as in Example 14, except that the mass ratio of the stems of Dendrobium officinale to the hydrangea was 6:1.
[0180] Comparative Example 2
[0181] The composition was prepared by the same method as in Example 18, except that the mass ratio of Dendrobium officinale stem to Hydrangea macrophylla was 1:6.
[0182] Comparative Example 3
[0183] The preparation method of the Dendrobium stem extract comprises:
[0184] (1) Raw material pretreatment: The Dendrobium officinale was weighed and crushed through an 80-mesh sieve.
[0185] (2) Extraction: Pure water was added to Dendrobium officinale at a solid-liquid ratio of 1:40 (m / m), stirred at room temperature for 30 min, extracted at 60° C. for 2 h, added with 0.5% activated carbon for deodorization, and then filtered through 200-mesh gauze to collect the filtrate.
[0186] (3) Membrane separation: The dendrobium filtrate was filtered using 10w and 50w membranes to collect the dendrobium polysaccharide extract with a molecular weight between 10w and 50wDa.
[0187] (4) Fine filtration: The coarse filtrate is cooled to below 35°C and filtered through H70 paperboard + red diatomaceous earth.
[0188] (5) Compounding: Add 23% glycerol to the refined filtrate to obtain a compound solution.
[0189] (6) Homogenization: The speed of the homogenizer for the compound liquid was 2500 rpm, and the homogenization was carried out for 10 min.
[0190] (7) Sterilization: Add 1% 1,2-pentanediol and 1.5% 1,2-hexanediol to the compound solution, sterilize with stirring at 98-100°C for 40 min, and cool to room temperature for storage.
[0191] Comparative Example 4
[0192] The preparation method of hydrangea extract comprises:
[0193] (1) Raw material pretreatment: Weigh the hydrangea and treat it under high temperature and high pressure (110°C, 10 min);
[0194] (2) Water was added in a ratio of 1:40 (m / m) to the hydrangea spore liquid, stirred at room temperature for 30 min, extracted at 60° C. for 2 h, added with 0.5% activated carbon for deodorization, filtered through 200-mesh gauze, and the filtrate was collected.
[0195] (3) Filtration: Filter the filtrate through F100 paperboard.
[0196] (4) Fine filtration: The coarse filtrate is cooled to below 35°C and filtered through H70 paperboard + red diatomaceous earth.
[0197] (5) Compounding: Add 23% glycerol to the refined filtrate to obtain a compound solution.
[0198] (6) Homogenization: The speed of the homogenizer for the compound liquid was 2500 rpm, and the homogenization was carried out for 10 min.
[0199] (7) Sterilization: Add 1% 1,2-pentanediol and 1.5% 1,2-hexanediol to the compound solution, sterilize with stirring at 98-100°C for 40 min, and cool to room temperature for storage.
[0200] Comparative Example 5
[0201] Commercially available sodium hyaluronate (commercially available product of Shandong Yinhe Biotechnology Co., Ltd.).
[0202] The following 27 cosmetic samples were prepared using the products of Examples 1 to 22 and Comparative Examples 1 to 5 and blank matrices for efficacy testing. The composition of the blank matrices is shown in Table 6.
[0203] Table 6 Blank matrix composition
[0204]
[0205] The method for preparing cosmetic samples includes:
[0206] (1) Group A: Add the powder into water, stir to dissolve and disperse, and heat to 80°C. Keep warm and stir until completely dissolved and uniformly dissolved. Keep warm and set aside.
[0207] (2) Cool down to 60°C, add Group B, and neutralize to a pH between 5.5 and 6.5;
[0208] (3) Cooling to 45° C., adding any sample of Examples 1 to 22 and Comparative Examples 1 to 4, and neutralizing to a pH of 5.5 to 6.5; wherein, when any sample of Examples 1 to 22 and Comparative Examples 1 to 4 is used to prepare a cosmetic sample, any sample of Examples 1 to 22 and Comparative Examples 1 to 4 accounts for 3% of the mass of the obtained cosmetic sample; when the sodium hyaluronate of Comparative Example 5 is used to prepare a cosmetic sample, the amount of sodium hyaluronate accounts for 1% of the mass of the obtained cosmetic sample (the maximum addition amount for leave-on cosmetics in the catalog (2021 edition) has been used);
[0209] (4) Cool down to 45°C, add Group C (pre-dissolved), and stir thoroughly to disperse.
[0210] It should be noted that the present invention only exemplarily lists the oil control effects of the cosmetic samples containing the products obtained from Examples 1 to 22 and Comparative Examples 1 to 4, each containing a lower content of 3 wt %. It can be understood that as the content of the composition of Examples 1 to 22 in the cosmetic samples increases, its efficacy is further improved accordingly.
[0211] Experimental Example 1
[0212] The present invention is exemplified by taking the application of the composition in the field of cosmetics as an example, and the oil control effect of the composition is verified through human efficacy tests.
[0213] 1. Subject recruitment
[0214] A total of 112 subjects were recruited.
[0215] 1.1 Inclusion criteria:
[0216] ①18 to 60 years old, healthy men or women, meeting the criteria for oily skin;
[0217] ② The skin T zone is oily (the oil content on the forehead before cleansing should not be less than 120μg / cm 2 );
[0218] ③ The skin moisture content is above 60 C.U. (excluding those with compensatory oil secretion due to dryness);
[0219] ④ Those who are willing to participate and can complete the required content according to the test requirements;
[0220] ⑤ Have not used products related to the tested efficacy in the past month, and have not received facial aesthetic treatments in the past 2 months;
[0221] ⑥ Those without severe systemic diseases, immunodeficiency or autoimmune diseases;
[0222] 7. Those without active allergic diseases;
[0223] ⑧ Those who have no history of allergy to skin care cosmetics;
[0224] 1.2 Exclusion criteria:
[0225] ① Those who do not meet the criteria for oily skin or those with severe acne;
[0226] ② Those who have participated in the test on oil control and its effect on skin condition within the last month;
[0227] ③People with skin allergic diseases;
[0228] ④People who are easily allergic to cosmetics;
[0229] ⑤ Those who have recently used hormone drugs and immunosuppressants;
[0230] ⑥Those with low degree of cooperation.
[0231] 2. Test site
[0232] On both sides of the forehead (the area from the eyebrow to the hairline, select 3 points at a distance of 2 cm from the midline).
[0233] 3. Usage:
[0234] Use on half of the face, once in the morning and once in the evening. After cleansing every day, use only this sample, 6 to 8 drops each time or adjust the number of drops according to your own situation, apply evenly on the face, wait for it to be absorbed, and collect oil data after continuous use for 1 month.
[0235] 4. Test Grouping
[0236] A total of 112 people were recruited, and 28 samples were randomly used on half of their faces. Each sample was used by 8 people.
[0237] 5. Index detection
[0238] Skin oil content
[0239] 6. Test sequence
[0240] Method: Use the specified facial cleanser to cleanse face (or sit for 1 hour) → test the skin oil content → group according to the test oil background value (the background value of each sample group is basically at the same level, and there is no significant difference) → distribute samples → use for 1 month → cleanse face (or sit for 1 hour) → test the skin oil content.
[0241] 7. Test Results
[0242] The room temperature of the test site is (25±1)℃, and the relative humidity is (40±5)%. The subjects should keep their bodies in a stable state before the test.
[0243] After cleansing and before using the samples, use the skin oil content tester Sebumeter to collect the oil content of the left and right foreheads, distribute samples, and use half of the face every morning and evening. After 1 month of continuous use, after cleansing the face with the cleansing product, use the skin oil content tester Sebumeter again to collect data from the test area and the control area, and use SPSS statistical software for t-test analysis.
[0244] The oil control effect of the oil control composition was evaluated by testing the change rate of oil content in the test area before and after use. The smaller the change rate value, the more obvious the reduction in skin oil content. The test results are shown in Table 7 below. In Table 7, each example corresponds to a cosmetic sample containing the composition of the example.
[0245] Table 7 Skin oil content and changes of cosmetic samples obtained from Examples 1 to 22 and Comparative Examples 1 to 5 before and after use
[0246]
[0247]
[0248] Note: *: compared with before use, P < 0.05; #: compared with the change rate of blank matrix, P < 0.05.
[0249] Please refer to Table 7. It can be seen from the data of Comparative Examples 3 to 5 that when the cosmetic sample contains only one of the substances among Dendrobium stem extract, Hydrangea extract and sodium hyaluronate, its oil control effect on the skin is significantly lower; and, combined with the data of Comparative Examples 1 and 2, it can be seen that even if the cosmetic sample contains Dendrobium stem (extract), Hydrangea (extract) and sodium hyaluronate at the same time, when the ratio of Dendrobium stem (extract) to Hydrangea (extract) is not within the scope of protection claimed by the present invention, its oil control effect is equivalent to the effect when the cosmetic sample contains only one of the substances among Dendrobium stem extract, Hydrangea extract and sodium hyaluronate, and the oil control effect is still poor.
[0250] The cosmetic samples prepared by the method containing Examples 1 to 22 showed a significant decrease in skin oil content before and after use (P < 0.05); and the cosmetic samples prepared by the method containing Examples 1 to 22 showed a much higher rate of change in skin oil content before and after use than the blank matrix, and much higher than the cosmetic samples containing the products obtained in Comparative Examples 1 to 5. Therefore, it can be seen from the data of Examples 1 to 22 and Comparative Examples 1 to 5 that when the ratio of Dendrobium stem (extract) and Hydrangea (extract) is maintained within the scope of the present invention, the oil control effect of the obtained composition can be significantly improved, and it has a good long-term oil control effect. In addition, it can be seen from the data of Examples 2, 6, 9, 12, and 16 that when the ratio of Dendrobium stem (extract) and Hydrangea (extract) is 4:3.5, its effect is more significant. In addition, the composition of the present invention is mild and non-irritating to the skin, and the participants feel good skin.
[0251] 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. Use of a composition containing a Dendrobium stem extract and a Hydrangea sphaerocephala extract in the preparation of cosmetics / medicines with oil-control effects.
2. The use according to claim 1, characterized in that: The composition comprises, by weight, 1 to 5 parts of a Dendrobium stem extract and 1 to 5 parts of a Hydrangea extract; Preferably, the composition comprises 3.5-4.5 parts of Dendrobium stem extract and 3-4 parts of Hydrangea extract in parts by weight; Preferably, the molecular weight of the dendrobium polysaccharide in the dendrobium stem extract is 10w-50wDa.
3. The use according to claim 1, characterized in that: The composition also includes sodium hyaluronate; Preferably, the amount of sodium hyaluronate is 0.05% to 0.5% by mass relative to the composition; Preferably, the amount of sodium hyaluronate is 0.1% to 0.2% by mass relative to the composition; Preferably, the mass ratio of the dendrobium polysaccharide in the dendrobium stem extract to the sodium hyaluronate is (1-6):
1.
4. The use according to claim 1, characterized in that: The preparation method of the composition comprises: The dendrobium stem and hydrangea are mixed and extracted with water as the extraction solvent at a solid-liquid ratio of 1:(10-80), and the extract is decolorized, deodorized and filtered.
5. The use according to claim 1, characterized in that: The preparation method of the composition comprises: (a) extracting, decolorizing, deodorizing, and filtering the stems of Dendrobium officinale using water as an extraction solvent at a solid-liquid ratio of 1:(10-80) to obtain a Dendrobium officinale polysaccharide extract; (b) extracting the hydrangea with a dendrobium polysaccharide extract and water at a solid-liquid ratio of 1:(10-100), and then decolorizing, deodorizing, and filtering the extract; Preferably, in step (a), the filtrate obtained by filtration is separated by membrane separation, and the filtrate with a molecular weight between 10w and 50wDa is collected to obtain the Dendrobium polysaccharide extract.
6. The use according to claim 1, characterized in that: The preparation method of the composition comprises: The dendrobium stem and hydrangea sphaerocephala are extracted respectively with water as the extraction solvent and the solid-liquid ratio being 1:(10-100), and the extract is decolorized, deodorized and filtered; then the dendrobium stem extract and the hydrangea sphaerocephala extract are mixed and compounded.
7. The use according to claim 6, characterized in that: The preparation method of the composition comprises: (a1) extracting, decolorizing, deodorizing, and filtering the stems of Dendrobium officinale using water as an extraction solvent at a solid-liquid ratio of 1:(10-80), separating the extract using a membrane separation method, and collecting the stem extract of Dendrobium officinale with a molecular weight between 10w and 50wDa; (b1) extracting the hydrangea with water at a solid-liquid ratio of 1:(10-80), and then decolorizing, deodorizing, and filtering the extract to obtain a hydrangea extract; (c1) mixing the Dendrobium stem extract and the Hydrangea macrophylla extract.
8. The use according to any one of claims 4 to 7, characterized in that: The extraction temperature is 40 to 90° C. and the extraction time is 1 to 4 hours. Preferably, the decolorization and deodorization comprises: adding activated carbon or hydrogen peroxide to the extract for treatment, and collecting the filtrate; Preferably, before the extraction, the hydrangea is subjected to high temperature micro-pressure or water vapor treatment.
9. The use according to any one of claims 3 to 7, characterized in that: The preparation method of the composition further comprises: mixing the mixture of the Dendrobium stem extract and the Hydrangea extract with sodium hyaluronate in proportion, and subjecting the mixture to homogenization, microwave, ultrasound and / or micro-pressure treatment; Preferably, the Dendrobium stem extract and sodium hyaluronate are mixed in proportion, homogenized, microwaved, ultrasonically and / or micro-pressured, and then mixed with the Hydrangea extract.
10. The use according to claim 9, characterized in that: The homogenization conditions include: a rotation speed of 2000 to 5000 rpm and a homogenization time of 5 to 30 minutes; Preferably, the micro-pressure conditions include: temperature of 110-121°C, gauge pressure of 0.05-0.13 MPa, and micro-pressure time of 5-20 min; Preferably, the microwave conditions include: microwave power of 200-800w, microwave time of 5-20min; Preferably, the ultrasonic conditions include: ultrasonic power of 50-400 W, ultrasonic temperature of 30-60° C., and ultrasonic time of 5-20 min.
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