Application of Dendrobium stem extract and Hydrangea extract in the preparation of cosmetics / pharmaceuticals
The composition of Dendrobium stem extract, Hydrangea extract and sodium hyaluronate solves the skin sensitivity and pore blockage problems of existing oil control products and achieves effective oil control effect.
Patent Information
- Application Number
- CN202411536290.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-31
- Publication Date
- 2025-09-23
- Estimated Expiration
- 2044-10-31
AI Technical Summary
Existing oil-control products have problems such as increased skin sensitivity, clogged pores, and limited oil-control capabilities, and their ingredients are numerous and complex.
A composition of a dendrobium stem extract and a hydrangea extract is combined with sodium hyaluronate in a specific ratio and extraction method to prepare cosmetics or medicines for oil control.
It achieves good oil control effect, reduces oil synthesis, relieves oily skin problems, and has simple ingredients, avoiding skin sensitivity and pore blockage.
Smart Images

Figure BDA0005111625130000151 
Figure BDA0005111625130000171 
Figure BDA0005111625130000181
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of skin care products, and in particular to the application of a dendrobium stem extract and a hydrangea extract in the preparation of cosmetics / medicines. Background Art
[0002] Oily skin is primarily caused by overactive sebaceous glands, which make it greasy and difficult to clean. This oiliness can also lead to acne, inflammation, and scaling. Therefore, controlling sebaceous gland secretion and reducing oil production is key to maintaining healthy and beautiful skin. The oil control market also has significant potential in terms of market share.
[0003] The causes of oily skin are related to the internal environment of the endocrine, nervous, and immune systems, and are also affected by many external factors such as diet. The main ones are: 1. Age: Newborns are affected by the androgen in their mothers' bodies, and the sebaceous glands are active. After puberty, the gonads and adrenal glands produce more androgens, the sebaceous glands enlarge, and the sebum increases. 2. Gender: After males enter puberty, the testicles begin to secrete androgen 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. It can maintain women's normal reproductive function and maintain the normal development of women's pubic hair, armpit hair, muscles and the whole body. Excessive androgen secretion in women can lead to increased oiliness in the skin, as androgen can inhibit the hypothalamus's secretion of gonadotropin-releasing hormone and counteract estrogen. ③ Endocrine: Androgen and adrenal cortex hormones in the human body can cause sebaceous gland hypertrophy and enhance secretory function. ④ Greasy, spicy, and high-sugar foods can generate heat in the spleen and stomach. Over time, this can lead to endogenous dampness and heat in the body, increasing sebum secretion. ⑤ Emotion: Emotions can stimulate the parasympathetic nervous system and endocrine system, which, through feedback, strengthens the endocrine system's secretion, increasing androgen secretion. Anxiety and staying up late can aggravate facial oiliness, among other factors. Many of the above factors can lead to oily skin.
[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. Currently, 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 spp. extract in the preparation of cosmetics / pharmaceuticals with oil-control efficacy.
[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 were mixed and extracted with water as the extraction solvent at a material-liquid ratio of 1:(10-80), and the extract was decolorized, deodorized and filtered.
[0015] In a specific embodiment of the present invention, the preparation method of the composition comprises:
[0016] (a) extracting the stems of Dendrobium officinale using water as an extraction solvent at a solid-liquid ratio of 1:(10-80), decolorizing and deodorizing, and filtering to obtain a Dendrobium officinale polysaccharide extract;
[0017] (b) extracting Hydrangea macrophylla with Dendrobium polysaccharide extract and water at a material-liquid ratio of 1:(10-100), and then decolorizing, deodorizing and filtering the extract.
[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 10wDa 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 are extracted separately with water as the extraction solvent and a solid-liquid ratio of 1:(10-100), and the extracts are decolorized, deodorized and filtered; and then the dendrobium stem extract and the hydrangea extract are mixed and compounded.
[0021] In a specific embodiment of the present invention, the preparation method of the composition comprises:
[0022] (a1) extracting the stems of Dendrobium officinale using water as an extraction solvent at a solid-liquid ratio of 1:(10-80), decolorizing and deodorizing, filtering, and separating the extract using a membrane separation method to collect the Dendrobium officinale stem extract 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 and deodorizing the extract and filtering it 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 spp. 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 spp. 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 minutes.
[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 to 400 W, ultrasonic temperature of 30 to 60° C., and ultrasonic time of 5 to 20 min.
[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 oleracea 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 resulting 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 understood 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 premise belong to the scope of protection of the present invention. Those who do not specify specific conditions in the embodiments are carried out according to normal conditions or the conditions recommended by the manufacturer. Those whose reagents or instruments are not specified by the manufacturer are 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 spp. extract in the preparation of cosmetics / pharmaceuticals with oil-control efficacy.
[0039] Dendrobium nobile Lindl. can nourish yin and eliminate heat. Modern pharmacology shows that Dendrobium 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 highest concentration among mushrooms. It also contains a variety of active ingredients, including protein, amino acids, and vitamins. Studies have shown that Sparassis crispa has a variety of benefits, including antioxidant activity, inhibition of inflammatory cytokine release, and regulation of the balance between 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. The composition has simple raw material types, can reduce oil synthesis, and effectively alleviate the problem of oily skin.
[0042] The composition containing the Dendrobium stem extract and the Hydrangea spp. extract of the present invention can be used in the preparation of cosmetics or pharmaceuticals. The cosmetics can be common types in the cosmetics field, such as lotions, emulsions, creams, facial masks, sunscreens, and makeup products, and can also be shampoos, bath products, and the like, and are not specifically limited. The type of pharmaceutical is also not specifically limited.
[0043] In a specific embodiment of the present invention, when preparing cosmetics or medicines, the composition is used in an amount ranging from 2 wt% to 50 wt%; preferably, it is used in an amount ranging from 2 wt% to 20 wt%; and more preferably, it is used in an amount ranging from 2.5 wt% to 10 wt%.
[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 spp. extract, based on weight parts.
[0045] For example, in different embodiments, the composition can include 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5 or 5 parts of Dendrobium stem extract, and can include 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5 or 5 parts of Hydrangea extract, and the amount of Dendrobium stem extract or Hydrangea extract can also be a number 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 chinensis extract is a water extract of Hydrangea chinensis.
[0049] In a specific embodiment of the present invention, the molecular weight of the dendrobium polysaccharide in the dendrobium stem extract is 10 wDa to 50 wDa. Maintaining the molecular weight of the dendrobium polysaccharide in the dendrobium stem extract within the above range can further enhance the oil control effect of the resulting composition.
[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.
[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 in parts by weight.
[0052] Monosaccharide molecules are the basic components of polysaccharides, which are formed through condensation and dehydration. Studies have shown that the functional activity of polysaccharides is directly and indirectly related to their monosaccharide composition. For example, the immunostimulatory and antioxidant activities of polysaccharides are affected by the relative content of monosaccharides. Analysis shows that the monosaccharide composition of the dendrobium polysaccharides in the dendrobium extract of the present invention is mainly composed of 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 spp. extract, and sodium hyaluronate, the oil-control effect of the composition is significantly further enhanced. The sodium hyaluronate can be prepared in-house or commercially available, such as that available from Shandong Galaxy Biotechnology Co., Ltd.
[0054] In a specific embodiment of the present invention, the amount of sodium hyaluronate used is 0.05 wt % to 0.5 wt % 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 1000 Da to 200 wDa.
[0058] For example, in different embodiments, the molecular weight of the sodium hyaluronate can be illustratively 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.
[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 a ratio between any two of the above ratios.
[0061] In a specific embodiment of the present invention, the composition further comprises an additive. Furthermore, 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 spp. extract.
[0067] In a specific embodiment of the present invention, the preparation method includes the following steps: using water as the extraction solvent and a solid-liquid ratio of 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 spp. In different embodiments, the solid-liquid ratio can be exemplified by 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), or a ratio between any two of the above ratios.
[0069] In a specific embodiment of the present invention, the preparation method includes the following steps: using water as the extraction solvent and extracting the dendrobium stem and hydrangea respectively at a solid-liquid ratio of 1:(10-100) (m / m), decolorizing and deodorizing the extract, and filtering; then mixing and compounding the dendrobium stem extract and the hydrangea extract.
[0070] In the above embodiment, water is used as the extraction solvent to extract the stems of Dendrobium and the hydrangea, respectively, to obtain the corresponding stem extracts of Dendrobium and the hydrangea, and then to mix and compound them. For example, in different embodiments, the material-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).
[0071] In a specific embodiment of the present invention, the preparation method comprises the following steps:
[0072] (a) extracting the stems of Dendrobium officinale with water as the extraction solvent at a solid-liquid ratio of 1:(10-80) (m / m), decolorizing and deodorizing, and filtering to obtain a Dendrobium officinale polysaccharide extract;
[0073] (b) extracting the hydrangea with the dendrobium polysaccharide extract and water at a material-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 to extract the stems of Dendrobium officinale first, and the stem extract of Dendrobium officinale is subjected to membrane separation to collect the Dendrobium officinale polysaccharide extract with a molecular weight between 10w and 50wDa; then the Dendrobium officinale polysaccharide extract and water are used as the extraction solvent to extract the hydrangea. For example, in different embodiments, in step (a), the material-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 material-liquid ratio refers to the mass 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 10wDa 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 the stems of Dendrobium officinale using water as an extraction solvent at a solid-liquid ratio of 1:(10-80) (m / m), decolorizing and deodorizing, filtering, and separating the extract using a membrane separation method to collect a Dendrobium officinale polysaccharide extract with a molecular weight between 10w and 50wDa;
[0079] (b1) extracting the hydrangea with water at a solid-liquid ratio of 1:(10-80) (m / m), and then decolorizing and deodorizing the extract and filtering it to obtain a hydrangea extract;
[0080] (c1) mixing the Dendrobium polysaccharide extract and the Hydrangea spp. extract.
[0081] In the above embodiment, water is used as an extraction solvent to first extract the stems of Dendrobium officinale, and the stem extract of Dendrobium officinale is subjected to membrane separation to collect a Dendrobium officinale polysaccharide extract with a molecular weight between 10w and 50wDa; then water is used as an extraction solvent to extract the Hydrangea spp. to obtain a Hydrangea spp. extract; and then the Dendrobium officinale polysaccharide extract and the Hydrangea spp. extract are compounded. For example, in different embodiments, in steps (a1) and (b1), the material-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.; and the extraction time is 1 to 4 hours.
[0083] For example, in different embodiments, the extraction temperature can be exemplified by 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 by 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 stems, or the mixture of the extraction solvent, the Dendrobium stems and the 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 process includes adding activated carbon or hydrogen peroxide to the extract, and collecting the filtrate. Furthermore, the activated carbon is added in an amount of 0.1% to 2% by weight of the extract, and the hydrogen peroxide is added in an amount of 0.01% to 1% by weight of the extract.
[0087] In a specific embodiment of the present invention, the hydrangea mushroom is subjected to high-temperature micro-pressure or steam treatment before extraction. Furthermore, 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 minutes; the steam treatment includes: steaming at 90-100°C for 5-20 minutes.
[0088] In a specific embodiment of the present invention, before the extraction, the stems of Dendrobium officinale are crushed and sieved to obtain the sieve residue.
[0089] In a specific embodiment of the present invention, the filtration process 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 cardboard filtration in the coarse filtration can be F100 cardboard 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 cardboard filtration can be H70 cardboard filtration.
[0091] In a specific embodiment of the present invention, the method for preparing the composition further comprises: mixing the mixture of the Dendrobium stem extract and the Hydrangea spp. extract with sodium hyaluronate in a proportional manner, and subjecting the mixture to homogenization, microwave treatment, ultrasound treatment, and / or micro-pressure treatment. In practice, sodium hyaluronate is added to the refined filtrate obtained by the filtration treatment; and a polyol such as glycerol is further added to 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 a certain proportion, homogenizing, microwave, ultrasonic and / or micro-pressure treating, and then mixing with the Hydrangea extract. The Dendrobium stem extract can 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 together with the seminal 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 2000-5000 rpm, and a homogenization time of 5-30 min; the micro-pressure conditions include: 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 microwave conditions include: a microwave power of 200-800 W, and a microwave time of 5-20 min; the ultrasonic conditions include: an ultrasonic power of 50-400 W, an ultrasonic temperature of 30-60° C., and an ultrasonic time of 5-20 min.
[0095] For example, in different embodiments, the speed of the homogenization can be exemplarily 2000rpm, 2200rpm, 2500rpm, 3000rpm, 3500rpm, 4000rpm, 4500rpm, 47rpm or 5000rpm, 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, 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, the process further includes: adding one or more of propylene glycol, butylene glycol, pentylene glycol, hexylene glycol or other polyols commonly used in cosmetics, and / or one or more of phenoxyethanol, ethylhexylglycerin or other preservatives commonly used in cosmetics to the compound 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] Examples 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 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. in 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 is completed, 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: a certain amount of glycerol is compounded 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), and sterilize by stirring at 80-100° C. (e.g., 98-100° C.) for 30-60 min (e.g., 40 min), and then 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] Examples 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 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 stems 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 is completed, 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 to the filtrate obtained in step (2) (all of the filtrate is used, and the rest is made up with water), and adding the hydrangea to the hydrangea at a material-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. and filtered through H70 paperboard + diatomaceous earth to collect the fine filtrate;
[0115] (5) Compounding: adding a certain amount of glycerol to the refined filtrate obtained in step (4) to obtain a compounded solution;
[0116] (6) Sterilization: Add 1,2-pentanediol and 1,2-hexanediol, or phenoxyethanol and ethylhexylglycerin to the compound solution of step (5), and sterilize by stirring at 80-100° C. (e.g., 98-100° C.) for 30-60 min (e.g., 40 min), and then 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] Examples 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 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 stems 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 is completed, add 0.1% to 2% activated carbon for decolorization and deodorization, then fine filter and collect the filtrate;
[0125] (3) membrane separation: the filtrate obtained in step (2) was filtered using a 10 wDa and a 50 wDa membrane to collect the Dendrobium polysaccharide extract with a molecular weight between 10 wDa and 50 wDa;
[0126] (4) adding 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 adding the hydrangea at a material-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; adding 0.1% to 2% activated carbon for decolorization and deodorization, and then filtering 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. and filtered through H70 paperboard + diatomaceous earth to collect the fine filtrate;
[0128] (6) Compounding: adding a certain amount of glycerol to 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 ethylhexylglycerin to the compound solution of step (6), and sterilize by stirring at 80-100° C. (e.g., 98-100° C.) for 30-60 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. in 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, then filter through 200-mesh gauze and collect the filtrate;
[0138] (3) Filtration: The filtrate from step (2) was filtered through F100 paperboard to collect the coarse filtrate; the coarse filtrate was then cooled to below 35°C and filtered through H70 paperboard + diatomaceous earth to collect the fine filtrate;
[0139] (4) Compounding: Compounding a certain amount of glycerol and 0.05% to 0.5% sodium hyaluronate with 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 minutes (e.g., 10 minutes);
[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% ethylhexylglycerin to the compound solution of step (4), and sterilize by stirring at 98 to 100° C. (e.g., 98 to 100° C.) for 30 to 60 minutes (e.g., 40 minutes), 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] Example 11 Example 12 Example 13 Example 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 glycerin 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] Examples 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 stems 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 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, then filter with 200-mesh gauze and 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 material-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: a certain amount of glycerol and 0.05% to 0.5% sodium hyaluronate are compounded into the refined filtrate of step (5) to obtain a compounded solution.
[0154] (7) Compound liquid treatment: Place the compound liquid of step (6) in a homogenizer and homogenize at a speed of 2000 to 5000 rpm (such as 2500 rpm) for 5 to 30 minutes (such as 10 minutes).
[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% ethylhexylglycerin to the reconstituted solution after treatment in step (7), and sterilize with stirring at 80 to 100° C. (e.g., 98 to 100° C.) for 30 to 50 minutes (e.g., 40 minutes), 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] Example 15 Example 16 Example 17 Example 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 glycerin 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] Example 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 micro-pressure (110°C, 20 min). Crush the stems of Dendrobium officinale and sieve them. The mass ratio of Dendrobium officinale stems to Hydrangea spp. is 4:3.5.
[0163] (2) Extraction: Weigh the stems 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) adding sodium hyaluronate to the dendrobium polysaccharide extract in step (3) to obtain a composite solution; placing the composite solution in a homogenizer and homogenizing at a speed of 2000 to 5000 rpm (e.g., 2500 rpm) for 5 to 30 minutes (e.g., 10 minutes).
[0166] (5) Extraction of Hydrangea: Hydrangea was stirred at room temperature for 30 min at a solid-liquid ratio of 1:60 (m / m), 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 (based on the 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 total mass of the Dendrobium polysaccharide extract in step (3), the hydrangea extract filtrate obtained in step (5) and the glycerol in step (6).
[0170] Example 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] Example 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] Example 22
[0177] This example refers to the preparation method of the composition of Example 15, with the only difference being that the hydrangea is not subjected to high-temperature micro-pressure treatment in step (1).
[0178] Comparative Example 1
[0179] The composition was prepared by the same method as in Example 14, except that the mass ratio of Dendrobium officinale stem to Hydrangea spp. 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: Crush the Dendrobium officinale and pass 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, and deodorized with 0.5% activated carbon. The mixture was then filtered through 200-mesh gauze and the filtrate was collected.
[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 10wDa 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 reconstituted 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 to the solution at a ratio of 1:40 (m / m) and the mixture was stirred at room temperature for 30 min. The mixture was extracted at 60°C for 2 h. 0.5% activated carbon was added for deodorization. The mixture was filtered through 200-mesh gauze and the filtrate was collected.
[0195] (3) Filtration: Filter the filtrate through F100 cardboard.
[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 reconstituted 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 preparation method of cosmetic samples includes:
[0206] (1) Group A: Add the powder to water, stir to dissolve and disperse, and heat to 80°C. Keep warm and stir until completely dissolved and uniform. Keep warm and set aside.
[0207] (2) Cool 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 one 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 one of Examples 1 to 22 and Comparative Examples 1 to 4 is used to prepare a cosmetic sample, any one 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℃, add Group C (pre-dissolved), stir and disperse thoroughly, and stir until evenly mixed.
[0210] It should be noted that the present invention only exemplifies the oil-control effects of the cosmetic samples containing the products of Examples 1 to 22 and Comparative Examples 1 to 4, each containing a relatively low content of 3 wt %. It is understandable that as the content of the composition of Examples 1 to 22 in the cosmetic samples increases, the efficacy thereof is further enhanced 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] ① Applicants aged 18 to 60 years old, healthy men or women, who meet the criteria for oily skin;
[0217] ② The skin's T-zone is oily (the oil content on the forehead before cleansing should not be less than 120μg / cm 2 );
[0218] ③ Skin moisture content is above 60 C.U. (excluding those with compensatory oil production 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 efficacy being tested in the past month, and have not received facial aesthetic treatments in the past two months;
[0221] ⑥ Those without severe systemic diseases, immunodeficiency or autoimmune diseases;
[0222] 7. Those without active allergic diseases;
[0223] ⑧ Those with no history of allergies 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 oil control and its impact on skin condition tests within the past month;
[0227] ③People with skin allergic diseases;
[0228] ④People who are allergic to cosmetics;
[0229] ⑤ Those who have recently used hormone drugs and immunosuppressants;
[0230] ⑥ Those with low cooperation degree.
[0231] 2. Test site
[0232] On both sides of the forehead (the area from above the eyebrows to the hairline, select 3 points at a distance of 2 cm from the midline).
[0233] 3. Instructions for use:
[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.Indicator detection
[0238] Skin oil content
[0239] 6. Test sequence
[0240] Methods: Use the specified facial cleanser to cleanse the face (or sit still for 1 hour) → test the skin oil content → group according to the tested 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 the face (or sit still 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 sample, use the skin oil content tester Sebumeter to collect the oil content of the left and right foreheads, distribute the sample, and use it on half of the face every morning and evening. After using it continuously for 1 month, after cleansing the face with the cleansing product and sitting still, use the skin oil content tester Sebumeter again to collect data from the test area and the control area respectively, and use SPSS statistical software for t-test analysis.
[0244] The oil-control effectiveness of the oil-control composition was evaluated by measuring the rate of change in oil content in the test area before and after use. A smaller rate of change indicates a more significant 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 that example.
[0245] Table 7 Skin oil content and changes before and after use of cosmetic samples obtained from Examples 1 to 22 and Comparative Examples 1 to 5
[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 using the methods 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 using the methods 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, based on the data of Examples 1 to 22 and Comparative Examples 1 to 5, it can be seen that when the ratio of Dendrobium stem (extract) and Hydrangea oleracea (extract) is maintained within the scope of the present invention, the oil control efficacy of the resulting 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 oleracea (extract) is 4:3.5, its efficacy is more significant. In addition, the composition of the present invention is mild and non-irritating to the skin, and the participants feel good about their 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 above embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the above 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 spp. extract in the preparation of cosmetics / pharmaceuticals with oil-control effects; the composition comprises, by weight, 1 to 5 parts of the Dendrobium stem extract and 1 to 5 parts of the Hydrangea spp. extract; 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, separating the filtrate obtained by filtration using a membrane separation method, and collecting the filtrate with a molecular weight between 10w and 50wDa 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 and deodorizing the extract and filtering it; or, (a1) extracting the stems of Dendrobium officinale using water as an extraction solvent at a solid-liquid ratio of 1:(10-80), decolorizing and deodorizing, filtering, and separating the extract using a membrane separation method to collect the Dendrobium officinale stem extract 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 and deodorizing the extract and filtering it to obtain a hydrangea extract; (c1) mixing the Dendrobium stem extract and the Hydrangea macrophylla extract.
2. The use according to claim 1, characterized in that In parts by weight, the composition comprises 3.5 to 4.5 parts of Dendrobium stem extract and 3 to 4 parts of Hydrangea spp. extract.
3. The use according to claim 1, characterized in that The molecular weight of the dendrobium polysaccharide in the dendrobium stem extract is 10w-50wDa.
4. The use according to claim 1, characterized in that The composition also includes sodium hyaluronate.
5. The use according to claim 4, characterized in that Calculated by mass percentage relative to the composition, the amount of sodium hyaluronate used is 0.05% to 0.5%.
6. The use according to claim 5, characterized in that Calculated by mass percentage relative to the composition, the amount of sodium hyaluronate used is 0.1% to 0.2%.
7. The use according to claim 4, characterized in that The mass ratio of the dendrobium polysaccharide in the dendrobium stem extract to the sodium hyaluronate is (1-6):
1.
8. The use according to claim 1, characterized in that The extraction temperature is 40-90° C.; the extraction time is 1-4 hours.
9. The use according to claim 1, characterized in that The decolorization and deodorization process includes: adding activated carbon or hydrogen peroxide to the extract for treatment, and collecting the filtrate.
10. The use according to claim 1, characterized in that Before the extraction, the hydrangea is subjected to high temperature micro-pressure or water vapor treatment.
11. The use according to any one of claims 4 to 7, characterized in that: The preparation method of the composition further comprises: mixing the mixture of the Dendrobium stem extract and the Hydrangea spp. extract with sodium hyaluronate in proportion, and performing homogenization, microwave, ultrasound and / or micro-pressure treatment.
12. The use according to claim 1, characterized in that The Dendrobium stem extract and sodium hyaluronate are mixed in proportion, homogenized, microwaved, ultrasonically and / or micro-pressed, and then mixed with the Hydrangea chinensis extract.
13. The use according to claim 11 or 12, characterized in that The homogenization conditions include: a rotation speed of 2000 to 5000 rpm and a homogenization time of 5 to 30 minutes.
14. The use according to claim 11 or 12, characterized in that: 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 minutes.
15. The use according to claim 11 or 12, characterized in that The microwave conditions include: microwave power of 200-800W, and microwave time of 5-20min.
16. The use according to claim 11 or 12, characterized in that The ultrasonic conditions include: ultrasonic power of 50 to 400 W, ultrasonic temperature of 30 to 60° C., and ultrasonic time of 5 to 20 minutes.
Citation Information
Patent Citations
Dendrobium candidum oil-control perfume
CN111956578A
Moisturizing composition as well as preparation method and application thereof
CN116509777A
Skin moistening composition, essence lotion and preparation method thereof
CN118267334A
Edible fungus fermentation filtrate and application thereof in shampoo product
CN118685460A