Anti-aging composition and application thereof

Abstract

The invention relates to an anti-aging composition and application thereof. The anti-aging composition is prepared from the following raw materials: dendrobium officinale, camellia japonica and polygonatum kingianum. Dendrobium officinale, camellia japonica and polygonatum kingianum cooperate with one another to achieve a synergistic effect, secretion of type I collagen (COL-1) can be promoted, secretion of matrix metalloproteinase-1 (MMP-1) can be inhibited, and decomposition of collagen in extracellular matrixes can be slowed down. The anti-aging composition can increase skin elasticity, improve the skin barrier function, reduce the percutaneous water loss rate and delay skin aging.

Description

Technical Field

[0001] The invention belongs to the technical field of cosmetics, and in particular relates to an anti-aging composition and application thereof. Background Art

[0002] Skin aging is a phenomenon of skin aging caused by natural and unnatural factors. Skin aging is mainly manifested in dry skin, decreased barrier function, roughness, decreased elasticity, wrinkles, and irregular pigmentation. There are many factors that cause skin aging, including ultraviolet rays, skin nutrient deficiency, oxygen free radicals, emotional stress, hormone secretion, etc. In addition to natural aging, there are many factors that cause skin aging. With the continuous improvement of people's awareness of skin care, "anti-aging" and "anti-early aging" are becoming more and more concerned and valued by people. People's demand for anti-aging products is increasing, and research on delaying skin aging is also gradually increasing.

[0003] CN118750408A discloses an anti-aging composition, comprising the following ingredients: Dendrobium officinale polysaccharide, superoxide dismutase, bifid yeast fermentation product lysate, stabilizer, butylene glycol, ethoxydiglycol, etc. The composition can remove free radicals, inhibit skin inflammation, repair damaged skin, promote the production of collagen in the skin, maintain the collagen content in the skin, and thus delay skin aging.

[0004] CN118593400A discloses an anti-aging composition, which specifically comprises the following raw materials: Bidens pilosa extract, snow tea leaf extract, Rosa roxburghii fruit extract, Phyllanthus emblica fruit extract, Viola extract, Tribulus terrestris fruit extract, Scrophularia ningpoensis extract and Bakuchiol. The composition delays skin aging by removing free radicals and increasing the water content of the stratum corneum.

[0005] Although removing skin free radicals can reduce collagen, there are many reasons for the decrease in collagen content in the skin, including decreased cell function and other external environmental factors. Currently, most anti-aging products are relatively single-minded and do not have the comprehensive effect of delaying skin aging.

[0006] Therefore, developing an anti-aging composition that can promote collagen growth in the skin in many aspects, reduce collagen degradation, ensure the continuous increase of collagen in the skin, enhance skin elasticity, and improve skin barrier function has become a technical problem that needs to be solved urgently. Summary of the invention

[0007] In view of the shortcomings of the prior art, the present invention aims to provide an anti-aging composition and its application. The components in the composition cooperate with each other to enhance synergy, promote COL-1 secretion, inhibit MMP-1 secretion, increase skin elasticity, and improve skin barrier function.

[0008] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0009] In a first aspect, the present invention provides an anti-aging composition, wherein raw materials for preparing the anti-aging composition include Dendrobium officinale, Camellia yunnanensis and Polygonatum cyrtonema.

[0010] Dendrobium candidum is a perennial epiphytic herb, which contains polysaccharides, flavonoids, phenols, amino acids and other substances, which have antioxidant, antibacterial, anti-inflammatory and other pharmacological activities. Yunnan Camellia contains not only natural germanium, selenium, molybdenum, vanadium, zinc, iron, calcium and other trace elements that can participate in the normal metabolism of the human body and have health-care effects, but also contains polyphenols, flavonoids, polysaccharides, triterpenoids, vitamins and other active ingredients, which have antioxidant, lipid-lowering, blood sugar-lowering, anti-tumor, moisturizing and whitening, detoxification and sore-healing, antibacterial and other effects. Yunnan Polygonatum is a perennial herb of the genus Polygonatum in the Liliaceae family, containing a variety of effective ingredients, such as polysaccharides, saponins, polyphenols, flavonoids, lignin and some anthraquinone compounds, which have the effects of lowering blood sugar, lowering lipids, anti-aging, anti-tumor, anti-virus, anti-osteoporosis and other effects.

[0011] The raw materials for preparing the anti-aging composition of the present invention include Dendrobium officinale, Camellia yunnanensis and Polygonatum yunnanensis, which work synergistically to promote the secretion of type I collagen (COL-1), inhibit the secretion of matrix metalloproteinase-1 (MMP-1), and slow down the decomposition of collagen in the extracellular matrix, thereby increasing skin elasticity, improving skin barrier function, and delaying skin aging.

[0012] Preferably, in parts by weight, the raw materials for preparing the anti-aging composition include 1 part of Dendrobium officinale, 1-10 parts of Camellia japonica, and 0.5-5 parts of Polygonatum sibiricum.

[0013] Among them, the specific point values ​​in 1 to 10 parts can be selected from 1 part, 3 parts, 5 parts, 7 parts, 9 parts, 10 parts, etc., and the specific point values ​​in 0.5 to 5 parts can be selected from 0.5 parts, 1 part, 2 parts, 3 parts, 4 parts, 5 parts, etc.

[0014] Based on the potential interaction between Dendrobium officinale, Camellia sinensis and Polygonatum sibiricum in anti-aging, when the three meet the above-mentioned specific proportion relationship, they can better promote collagen production and achieve the effect of delaying skin aging.

[0015] Preferably, the anti-aging composition is prepared by a preparation method comprising the following steps:

[0016] (1) mixing the raw materials for preparing the anti-aging composition with a solvent and performing hot reflux extraction to obtain a crude extract;

[0017] (2) mixing the crude extract with the composite enzyme to perform an enzymatic hydrolysis reaction to obtain an enzymatic hydrolysis product;

[0018] (3) The enzymatic hydrolysis product is subjected to flocculation treatment and purification to obtain the anti-aging composition.

[0019] Preferably, the step (1) further comprises subjecting the prepared raw materials to ultra-high pressure treatment before the hot reflux extraction.

[0020] In the present invention, the raw materials are subjected to ultra-high pressure treatment before hot reflux extraction, so that the cell structure of the raw materials is changed. The obtained anti-aging composition has a higher content of active ingredients, which can ensure the anti-aging effect to a greater extent.

[0021] Preferably, the pressure of the ultra-high pressure treatment is 200-350 MPa, and the holding time is 5-15 min.

[0022] Among them, the specific point values ​​in 200-350MPa can be selected as 200MPa, 240MPa, 280MPa, 320MPa, 350MPa, and the specific point values ​​in 5-15min can be selected as 5min, 7min, 9min, 11min, 13min, 15min, etc.

[0023] When the above-mentioned specific process parameters are selected for ultrahigh pressure treatment, the extraction efficiency of active ingredients in the preparation raw materials can be further improved.

[0024] Preferably, the number of times of the hot reflux extraction in step (1) is 1 to 4 times, and the time of each hot reflux extraction is 1 to 3 hours.

[0025] Among them, the specific point values ​​in 1 to 4 times can be selected as 1 time, 2 times, 3 times, 4 times, etc., and the specific point values ​​in 1 to 3h can be selected as 1h, 1.5h, 2h, 2.5h, 3h, etc.

[0026] Preferably, the solvent comprises an aqueous solution of ethanol.

[0027] In the present invention, the ethanol extracts of Dendrobium officinale, Camellia japonica and Polygonatum cyrtonema are obtained by extracting the raw materials with an ethanol aqueous solution, which can better promote the secretion of COL-1, inhibit the secretion of MMP-1, and exert the anti-aging effect of the composition.

[0028] Preferably, the volume percentage of ethanol in the ethanol aqueous solution is 50-80%, for example, 50%, 60%, 70%, 80%, etc.

[0029] Preferably, the complex enzyme in step (2) comprises papain, cellulase and pectinase.

[0030] Papain can hydrolyze protein, help decompose the protein components in the raw materials, and release related active peptides; cellulase can decompose cellulose, and pectinase can decompose pectin. The synergistic effect of papain, cellulase and pectinase can help decompose the protein, cellulose, pectin and other raw materials in the preparation into small molecular active peptides, polysaccharides and other active ingredients, thereby enhancing the anti-aging effect of the composition.

[0031] Preferably, the mass ratio of papain, cellulase and pectinase is 1:(1-10):(0.5-10).

[0032] Among them, the specific point values ​​​​from 1 to 10 can be selected from 1, 3, 5, 7, 9, 10, etc., and the specific point values ​​​​from 0.5 to 10 can be selected from 0.5, 1, 3, 5, 7, 9, 10, etc.

[0033] Preferably, the mass ratio of the crude extract to the complex enzyme is (30-100):1.

[0034] Among them, the specific point values ​​between 30 and 100 can be selected from 30, 40, 50, 60, 70, 80, 90, 100, etc.

[0035] Preferably, the temperature of the enzymatic hydrolysis reaction is 20-50° C., and the time is 0.5-2 h.

[0036] Among them, the specific point values ​​in 20-50°C can be selected from 20°C, 30°C, 40°C, 50°C, etc., and the specific point values ​​in 0.5-2h can be selected from 0.5h, 1h, 1.5h, 2h, etc.

[0037] Preferably, the flocculation treatment in step (3) comprises mixing the enzymatic hydrolysis product with a flocculant for flocculation treatment;

[0038] Preferably, the flocculant comprises any one of sodium alginate, guar gum or gelatin, or a combination of at least two of them.

[0039] Sodium alginate is a sodium salt of a polyanionic polysaccharide extracted from kelp or sargassum of brown algae. It has good adsorption, stability, flocculation and chelating properties. Guar gum is a natural high-molecular plant gum that can adsorb and condense impurity particles in the solution and promote the sedimentation of impurities. Bone glue is an animal glue and a high-molecular substance. After being added to water, it promotes the aggregation of destabilized colloidal particles through adsorption and bridging.

[0040] Preferably, the flocculant comprises sodium alginate, guar gum and gelatin.

[0041] The three components cooperate with each other to achieve a better flocculation effect, and have a better effect in increasing the content of the effective ingredients in the composition.

[0042] Preferably, the mass ratio of the sodium alginate, guar gum and gelatin is 1:(1-5):(1-3).

[0043] Among them, the specific point values ​​1 to 5 can be selected from 1, 2, 3, 4, 5, etc., and the specific point values ​​1 to 3 can be selected from 1, 1.5, 2, 2.5, 3, etc.

[0044] Preferably, the mass of the flocculant is 0.1% to 2% of the mass of the enzymatic hydrolysis product, for example, it can be 0.1%, 0.5%, 1%, 1.5%, 2%, etc.

[0045] Preferably, after the flocculation treatment in step (3), activated carbon is added for decolorization.

[0046] Preferably, the purification in step (3) comprises purifying with a macroporous resin and eluting with water and an aqueous solution of ethanol in sequence, and collecting the aqueous solution of ethanol.

[0047] Preferably, the type of the macroporous resin includes any one of type D101, type DM301 or type AB-8, or a combination of at least two of them.

[0048] Preferably, the macroporous resin includes D101 type and DM301 type.

[0049] D101 macroporous resin is a styrene-type non-polar copolymer, and DM301 macroporous resin is a styrene-type medium-polar copolymer. In the present invention, when D101 and DM301 macroporous resins are selected for doping, multiple active ingredients can be adsorbed and separated in a targeted manner, thereby improving the selectivity and effect of purification, thereby better exerting the anti-aging effect of the composition.

[0050] Preferably, the flow rate of eluting with water is 0.5 to 2 BV / h, and the amount used is 1 to 3 BV.

[0051] Preferably, the flow rate of elution with the ethanol aqueous solution is 0.5 to 2 BV / h, and the amount used is 1 to 3 BV.

[0052] Among them, the specific point values ​​in 0.5~2BV / h can be selected from 0.5BV / h, 1BV / h, 1.5BV / h, 2BV / h, etc., and the specific point values ​​in 1~3BV can be selected from 1BV, 1.5BV, 2BV, 2.5BV, 3BV, etc.

[0053] Preferably, when eluting with an aqueous solution of ethanol, the volume percentage of ethanol in the aqueous solution of ethanol is 50% to 65%, for example, it can be 50%, 55%, 60%, 65%, etc.

[0054] Preferably, the purification in step (3) further comprises concentration and drying.

[0055] Preferably, the concentrating comprises concentrating under reduced pressure.

[0056] Preferably, the drying comprises freeze drying or spray drying.

[0057] In a second aspect, the present invention provides a use of the anti-aging composition as described in the first aspect in cosmetics.

[0058] The numerical range described in the present invention not only includes the point values ​​listed above, but also includes any point values ​​between the above numerical ranges that are not listed. Due to space limitations and for the sake of simplicity, the present invention no longer exhaustively lists the specific point values ​​included in the range.

[0059] Compared with the prior art, the present invention has the following beneficial effects:

[0060] The anti-aging composition provided by the present invention has three raw materials, namely, Dendrobium officinale, Camellia yunnanensis and Polygonatum yunnanensis, which cooperate with each other to enhance the effect synergistically, can promote the secretion of type I collagen, inhibit the secretion of matrix metalloproteinase-1, slow down the decomposition of collagen in the extracellular matrix, thereby increasing skin elasticity, improving skin barrier function and delaying skin aging.

[0061] Furthermore, in the preparation process of the anti-aging composition, ultra-high pressure treatment of the preparation raw materials before hot reflux extraction can increase the content of active ingredients in the prepared anti-aging composition and ensure the anti-aging effect of the composition to a greater extent.

[0062] Furthermore, during the preparation of the anti-aging composition, the crude extract is mixed with a composite enzyme for enzymatic hydrolysis. The synergistic effect of papain, cellulase and pectinase in the composite enzyme can help release the active ingredients in the raw materials, thereby enhancing the anti-aging effect of the composition.

[0063] Furthermore, after enzymatic hydrolysis, sodium alginate, guar gum and gelatin are used as flocculants to flocculate the enzymatic hydrolysis product. The three flocculants cooperate with each other to achieve a better flocculation effect, which has a better effect in increasing the content of the effective ingredients in the composition.

[0064] Furthermore, in the preparation process of the anti-aging composition, D101 and DM301 macroporous resins are selected for doping and purification, which can specifically adsorb and separate a variety of effective ingredients, improve the selectivity and effect of purification, and thus better exert the anti-aging effect of the composition. DETAILED DESCRIPTION

[0065] In order to further explain the technical means and effects adopted by the present invention, the technical solution of the present invention is further described below in conjunction with the preferred embodiments of the present invention, but the present invention is not limited to the scope of the embodiments.

[0066] The sources of the components / raw materials in the following embodiments are shown in Table 1:

[0067] Table 1

[0068] Components / Raw Materials factory Brand Dendrobium officinale Yunnan Daocheng Chinese Medicinal Herbs Planting Co., Ltd. / Camellia yunnanensis Yunnan Daocheng Chinese Medicinal Herbs Planting Co., Ltd. / Polygonatum yunnanensis Yunnan Daocheng Chinese Medicinal Herbs Planting Co., Ltd. / Papain Shifeng Bio Enzyme activity 100U / mg Cellulase Shifeng Bio Enzyme activity 400U / mg Pectinase Shifeng Bio Enzyme activity 60U / mg Sodium alginate Qingdao Mingyue Seaweed Group Co., Ltd. HYF Guar Gum Shandong Xinghongsheng Biotechnology Co., Ltd. F-21 bone glue Zhengzhou Xinke Chemical Products Co., Ltd. / Polydimethylsiloxane Dow Corning PMX200 / 350CS Hyaluronic acid Bloomage Biopharmaceuticals HA-TP

[0069] Example 1

[0070] This embodiment provides an anti-aging composition, which is prepared by the following method:

[0071] (1) 181.8 g of Dendrobium candidum, 600 g of Camellia sinensis, and 218.2 g of Polygonatum cyrtonema were crushed into 50 meshes, and then subjected to ultrahigh pressure treatment at a pressure of 250 MPa and a holding time of 10 min to obtain a treated product. 6000 g of 70% ethanol aqueous solution was added to the treated product, and hot reflux extraction was performed for 2 h, and the extraction was performed 3 times. The extracts from the 3 times were combined and concentrated under reduced pressure to 1000 g to obtain a crude extract.

[0072] (2) 1000 g of the crude extract was mixed with 20 g of a composite enzyme (2 g of papain, 10 g of cellulase and 8 g of pectinase), and the mixture was reacted at 35° C. for 1 h to obtain an enzymatic hydrolysis product.

[0073] (3) Take 10 g of a flocculant (composed of 1 part of sodium alginate, 3 parts of guar gum and 2 parts of gelatin by weight), heat and dissolve the flocculant with water, cool it, mix it with 1000 g of the enzymatic hydrolysate, stir it at 35°C for 1 hour for flocculation treatment, centrifuge it at 2000 rpm for 40 minutes, take the supernatant and add 10 g of activated carbon for decolorization treatment, filter to remove the activated carbon, and obtain a filtrate.

[0074] (4) The decolorized filtrate is purified by adding 1500 g of macroporous resin (doped with 700 g of D101 macroporous resin and 800 g of DM301 macroporous resin), firstly washed with water (the amount of water is 2 BV, and the flow rate is 1.5 BV / h), and then washed with 65% ethanol aqueous solution (the amount of ethanol aqueous solution is 2 BV, and the flow rate is 1.5 BV / h), and the ethanol aqueous solution fraction is collected and concentrated under reduced pressure until there is no ethanol smell, and the concentrate is spray-dried to obtain an anti-aging composition.

[0075] Example 2

[0076] This embodiment provides an anti-aging composition, which is prepared by the following method:

[0077] (1) 100 g of Dendrobium candidum, 500 g of Camellia sinensis, and 400 g of Polygonatum cyrtonema were crushed into 70 meshes, and then subjected to ultrahigh pressure treatment at a pressure of 300 MPa and a holding time of 6 min to obtain a treated product. 4000 g of 80% ethanol aqueous solution was added to the treated product, and hot reflux extraction was performed for 3 h, and the extraction was performed twice. The extracts from the two times were combined and concentrated under reduced pressure to 1000 g to obtain a crude extract.

[0078] (2) 1000 g of the crude extract was mixed with 15 g of a composite enzyme (3 g of papain, 5 g of cellulase and 7 g of pectinase), and the mixture was reacted at 40° C. for 1 h to obtain an enzymatic hydrolysis product.

[0079] (3) Take 5 g of a flocculant (composed of 2 parts of sodium alginate, 2 parts of guar gum and 2 parts of gelatin by weight), heat and dissolve the flocculant with water, cool it, mix it with 1000 g of the enzymatic hydrolysate, stir it at 30°C for 1.5 h for flocculation treatment, centrifuge it at 3000 rpm for 20 min, take the supernatant and add 7 g of activated carbon for decolorization treatment, filter to remove the activated carbon, and obtain a filtrate.

[0080] (4) The decolorized filtrate is purified by adding 1200 g of macroporous resin (doped with 500 g of D101 macroporous resin and 700 g of DM301 macroporous resin), firstly washed with water (the amount of water is 1.5 BV, and the flow rate is 1 BV / h), and then washed with 60% ethanol aqueous solution (the amount of ethanol aqueous solution is 1.5 BV, and the flow rate is 1 BV / h), collecting the ethanol aqueous solution fraction, and concentrating it under reduced pressure until there is no ethanol smell, and spray drying the concentrate to obtain an anti-aging composition.

[0081] Example 3

[0082] This embodiment provides an anti-aging composition, which is prepared by the following method:

[0083] (1) 100 g of Dendrobium candidum, 350 g of Camellia yunnanensis, and 550 g of Polygonatum yunnanensis were crushed into 60 meshes, and then subjected to ultrahigh pressure treatment at a pressure of 200 MPa and a holding time of 15 min to obtain a treated product. 8000 g of 60% ethanol aqueous solution was added to the treated product, and hot reflux extraction was performed for 2 h, and the extraction was performed 4 times. The extracts obtained from the 4 times were combined and concentrated under reduced pressure to 1000 g to obtain a crude extract.

[0084] (2) 1000 g of the crude extract was mixed with 30 g of a composite enzyme (4 g of papain, 15 g of cellulase and 11 g of pectinase), and the mixture was reacted at 30° C. for 1 h to obtain an enzymatic hydrolysis product.

[0085] (3) Take 15 g of a flocculant (composed of 1 part of sodium alginate, 2 parts of guar gum and 3 parts of gelatin by weight), heat and dissolve the flocculant with water, cool it, mix it with 1000 g of the enzymatic hydrolysate, stir it at 40°C for 1 h for flocculation treatment, centrifuge it at 2500 rpm for 30 min, take the supernatant and add 5 g of activated carbon for decolorization treatment, filter to remove the activated carbon, and obtain a filtrate.

[0086] (4) The decolorized filtrate is purified by adding 1000 g of macroporous resin (doped with 600 g of D101 macroporous resin and 400 g of DM301 macroporous resin), first washed with water (the amount of water is 3 BV, the flow rate is 2 BV / h), and then washed with 50% ethanol aqueous solution (the amount of ethanol aqueous solution is 3 BV, the flow rate is 2 BV / h), collecting the ethanol aqueous solution fraction, concentrating under reduced pressure until there is no ethanol smell, and spray drying the concentrate to obtain an anti-aging composition.

[0087] Example 4

[0088] This embodiment provides an anti-aging composition, which differs from Embodiment 1 only in that the ultrahigh pressure treatment in step (1) is not performed, that is, 181.8 g of Dendrobium officinale, 600 g of Camellia japonica, and 218.2 g of Polygonatum cyrtonema are crushed into 50 mesh, and 6000 g of 70% ethanol aqueous solution are added for hot reflux extraction.

[0089] Example 5

[0090] This embodiment provides an anti-aging composition, which differs from Embodiment 1 only in that the 20 g of compound enzyme (2 g of papain, 10 g of cellulase and 8 g of pectinase) in step (2) is replaced by 20 g of compound enzyme (3.33 g of papain and 16.67 g of cellulase).

[0091] Example 6

[0092] This embodiment provides an anti-aging composition, which differs from Embodiment 1 only in that the 20 g of compound enzyme (2 g of papain, 10 g of cellulase and 8 g of pectinase) in step (2) is replaced by 20 g of compound enzyme (4 g of papain and 16 g of pectinase).

[0093] Example 7

[0094] This embodiment provides an anti-aging composition, which differs from Embodiment 1 only in that the 20 g of compound enzyme (2 g of papain, 10 g of cellulase and 8 g of pectinase) in step (2) is replaced by 20 g of compound enzyme (11.11 g of cellulase and 8.89 g of pectinase).

[0095] Example 8

[0096] This embodiment provides an anti-aging composition, which differs from Embodiment 1 only in that 10 g of flocculant (composed by weight of 1 part of sodium alginate, 3 parts of guar gum and 2 parts of gelatin) in step (3) is replaced by 10 g of flocculant (composed by weight of 1.5 parts of sodium alginate and 4.5 parts of guar gum).

[0097] Example 9

[0098] This embodiment provides an anti-aging composition, which differs from Embodiment 1 only in that 10 g of flocculant (composed of 1 part of sodium alginate, 3 parts of guar gum and 2 parts of gelatin by weight) in step (3) is replaced by 10 g of flocculant (composed of 2 parts of sodium alginate and 4 parts of gelatin by weight).

[0099] Example 10

[0100] This embodiment provides an anti-aging composition, which differs from Embodiment 1 only in that 10 g of flocculant (composed of 1 part of sodium alginate, 3 parts of guar gum and 2 parts of gelatin by weight) in step (3) is replaced by 10 g of flocculant (composed of 3.6 parts of guar gum and 2.4 parts of gelatin by weight).

[0101] Embodiment 11

[0102] This embodiment provides an anti-aging composition, which differs from Embodiment 1 only in that 1500 g of macroporous resin (700 g of D101 macroporous resin and 800 g of DM301 macroporous resin mixed) in step (4) is replaced by 1500 g of D101 macroporous resin.

[0103] Example 12

[0104] This embodiment provides an anti-aging composition, which differs from Embodiment 1 only in that 1500 g of macroporous resin (700 g of D101 macroporous resin and 800 g of DM301 macroporous resin mixed) in step (4) is replaced by 1500 g of DM301 macroporous resin.

[0105] Example 13

[0106] This embodiment provides an anti-aging composition, which is prepared by the following method:

[0107] (I) Preparation of Dendrobium officinale extract:

[0108] (1) 1000 g of Dendrobium officinale was crushed into 50 meshes, and then subjected to ultrahigh pressure treatment at a pressure of 250 MPa and a holding time of 10 min to obtain a treated product. 6000 g of 70% ethanol aqueous solution was added to the treated product, and hot reflux extraction was performed for 2 h, and the extraction was performed 3 times. The extracts from the 3 times were combined and concentrated under reduced pressure to 1000 g to obtain a crude extract.

[0109] (2) 1000 g of the crude extract was mixed with 20 g of a composite enzyme (2 g of papain, 10 g of cellulase and 8 g of pectinase), and the mixture was reacted at 35° C. for 1 h to obtain an enzymatic hydrolysis product.

[0110] (3) Take 10 g of a flocculant (composed of 1 part of sodium alginate, 3 parts of guar gum and 2 parts of gelatin by weight), heat and dissolve the flocculant with water, cool it, mix it with 1000 g of the enzymatic hydrolysate, stir it at 35°C for 1 hour for flocculation treatment, centrifuge it at 2000 rpm for 40 minutes, take the supernatant and add 10 g of activated carbon for decolorization treatment, filter to remove the activated carbon, and obtain a filtrate.

[0111] (4) The decolorized filtrate was purified by adding 1500 g of macroporous resin (doped with 700 g of D101 macroporous resin and 800 g of DM301 macroporous resin), first washed with water (the amount of water was 2 BV, and the flow rate was 1.5 BV / h), and then washed with 65% ethanol aqueous solution (the amount of ethanol aqueous solution was 2 BV, and the flow rate was 1.5 BV / h), and the ethanol aqueous solution fraction was collected and concentrated under reduced pressure until there was no ethanol taste, and the concentrated solution was spray-dried to obtain the Dendrobium officinale extract.

[0112] (II) Preparation of Camellia sinensis extract:

[0113] The preparation method of the Yunnan Camellia extract refers to the preparation method of the Dendrobium Officinale extract in step (I), and the only difference between it and step (I) is that 1000 g of Dendrobium Officinale is replaced by 1000 g of Yunnan Camellia.

[0114] (III) Preparation of Polygonatum odoratum extract:

[0115] The preparation method of the Yunnan polygonatum sibiricum extract refers to the preparation method of the Dendrobium officinale extract in step (I), and the only difference between it and step (I) is that 1000 g of Dendrobium officinale is replaced by 1000 g of Yunnan polygonatum sibiricum.

[0116] (IV) The Dendrobium officinale extract, Camellia japonica extract and Polygonatum cyrtonema extract prepared in steps (I) to (III) are mixed in a mass ratio of 1:3.3:1.2 to obtain an anti-aging composition.

[0117] Comparative Example 1

[0118] This comparative example provides an anti-aging composition, which differs from Example 1 only in that 181.8 g of Dendrobium officinale, 600 g of Camellia japonica, and 218.2 g of Polygonatum cyrtonema in step (1) are replaced with 232.5 g of Dendrobium officinale and 767.5 g of Camellia japonica.

[0119] Comparative Example 2

[0120] This comparative example provides an anti-aging composition, which differs from Example 1 only in that 181.8 g of Dendrobium officinale, 600 g of Camellia japonica, and 218.2 g of Polygonatum sibiricum in step (1) are replaced with 454.5 g of Dendrobium officinale and 545.5 g of Polygonatum sibiricum.

[0121] Comparative Example 3

[0122] This comparative example provides an anti-aging composition, which differs from Example 1 only in that 181.8 g of Dendrobium officinale, 600 g of Camellia japonica, and 218.2 g of Polygonatum cyrtonema in step (1) are replaced with 733.3 g of Camellia japonica and 266.7 g of Polygonatum cyrtonema.

[0123] Comparative Example 4

[0124] This comparative example provides an anti-aging composition, which differs from Example 1 only in that 181.8 g of Dendrobium officinale, 600 g of Camellia japonica, and 218.2 g of Polygonatum sibiricum in step (1) are replaced with 1000 g of Dendrobium officinale.

[0125] Comparative Example 5

[0126] This comparative example provides an anti-aging composition, which differs from Example 1 only in that 181.8 g of Dendrobium officinale, 600 g of Camellia japonica, and 218.2 g of Polygonatum cyrtonema in step (1) are replaced with 1000 g of Camellia japonica.

[0127] Comparative Example 6

[0128] This comparative example provides an anti-aging composition, which differs from Example 1 only in that 181.8 g of Dendrobium officinale, 600 g of Camellia japonica, and 218.2 g of Polygonatum sibiricum in step (1) are replaced with 1000 g of Polygonatum sibiricum.

[0129] Application Example 1

[0130] This application example provides an emulsion, which includes, by mass percentage, 1% of the anti-aging composition prepared in Example 1, 10% of polydimethylsiloxane, 4% of squalane, 5% of isohexadecane, 3% of glycerol, 5% of butylene glycol, 3% of hyaluronic acid, 5% of glyceryl stearate, and the balance is water.

[0131] Application Examples 2 to 13

[0132] Application Examples 2 to 13 each provide an emulsion, which differs from Application Example 1 only in that the anti-aging composition prepared in Example 1 is replaced by an anti-aging composition prepared in Examples 2 to 13 of equal mass.

[0133] Comparative Application Examples 1 to 6

[0134] Comparative Application Examples 1 to 6 each provide an emulsion, which differs from Application Example 1 only in that the anti-aging composition prepared in Example 1 is replaced with an anti-aging composition prepared in Comparative Examples 1 to 6 of equal mass.

[0135] Test Example 1

[0136] Testing the anti-aging composition for H 2 O 2 Effect of induced oxidative stress on the secretion of COL-1 and MMP-1 by HDF cells

[0137] (1) Preparation of samples to be tested:

[0138] Take 320 mg of the anti-aging composition prepared in Examples 1 to 13 and Comparative Examples 1 to 6 respectively, add distilled water to prepare 800 mg / L of the test samples Examples 1 to 13 and the test samples Comparative Examples 1 to 6.

[0139] (2) Obtaining HDF cells under oxidative stress and experimental grouping

[0140] Experimental Group:

[0141] ① Take the qualified HDF cells of the third generation after digestion, collect the cells, and resuspend them in serum-free DMEM culture medium (cell density 1×10 5 cells / mL) and then inoculated into a 96-well plate at 100 μL per well and placed in an incubator for 12 h to allow the cells to adhere to the wall;

[0142] ②Replace with fresh serum-free DMEM culture medium (200 μL per well), incubate in the incubator for 24 h, and add 200 μL of 200 μM H prepared in DMEM culture medium to each well. 2 O 2 , and continued incubation for 24 h to obtain HDF cells in an oxidative stress state;

[0143] ③ Add 200 μL of the test substances of Examples 1 to 13 and Comparative Examples 1 to 6 at a concentration of 50 mg / ml (prepared in DMEM culture medium) and incubate for 48 h;

[0144] H 2 O 2 Group:

[0145] The only difference between the treatment steps of the experimental group and the control group was that 200 μL of DMEM culture medium was added in step ③ and incubated for 48 h;

[0146] Blank control group:

[0147] The difference between the treatment steps of the experimental group and the experimental group is that the treatment of step ② is not performed, and 200 μL DMEM culture medium is added after the cells adhere to the wall and incubated for 48 hours.

[0148] (3) Test of COL-1 and MMP-1 secretion by HDF cells under oxidative stress

[0149] The culture supernatant of each group was collected and centrifuged. The test operation was carried out according to the instructions of the ELISA kit. The absorbance value of each well was detected by an enzyme marker, with 450nm as the detection wavelength and 630nm as the reference wavelength. The test results are shown in Table 2:

[0150] Table 2

[0151] Test substance Relative secretion of COL-1 Relative secretion of MMP-1 Blank control group 100.00 100.00 <![CDATA[H 2 O 2 group]]> 54.55 146.18 Example 1 119.76 77.48 Example 2 111.29 86.84 Example 3 111.78 87.53 Example 4 107.59 95.75 Example 5 104.96 90.10 Example 6 108.76 89.41 Example 7 105.30 90.44 Example 8 108.95 89.93 Example 9 109.68 90.27 Example 10 107.98 90.96 Embodiment 11 110.27 92.84 Example 12 99.37 90.44 Example 13 110.85 89.76 Comparative Example 1 91.53 104.15 Comparative Example 2 90.75 107.91 Comparative Example 3 86.76 116.82 Comparative Example 4 82.63 121.27 Comparative Example 5 83.26 123.67 Comparative Example 6 85.60 122.13

[0152] Test Example 2

[0153] Skin elasticity test

[0154] 95 women were selected as subjects and divided into 19 groups, with 5 people in each group. A half-face control test was carried out at the same time. According to the use requirements, the test side emulsion prepared by Application Examples 1 to Application Examples 13 and Comparative Application Examples 1 to 6 was used on the entire half of the face, and the blank control side emulsion was used on the other half of the face (the blank control side emulsion, calculated by mass percentage, includes 10% polydimethylsiloxane, 4% squalane, 5% isohexadecane, 3% glycerol, 5% butylene glycol, 3% hyaluronic acid, 5% glyceryl stearate, and the balance is water).

[0155] Apply once a day for 28 consecutive days, and collect data on both sides of the face on the 0th day (before use) and the 28th day of continuous use.

[0156] The skin elasticity was tested using the German CK company's skin elasticity tester Cutometer MPA580. The test principle is based on the suction and stretching principle. A negative pressure is generated on the surface of the tested skin to suck the skin into a specific test probe. The depth of the skin sucked into the test probe is measured by a non-contact optical test system. The skin elasticity value R2 is calculated from the measured value. The larger the R2 value, the better the skin elasticity. The test results of each test group are averaged, and the results are shown in the following table:

[0157] Table 3

[0158]

[0159]

[0160] Test Example 3

[0161] Transepidermal water loss test

[0162] The same batch of 95 subjects from Test Example 2 were selected and the following transepidermal water loss test was performed on the subjects: the test area was randomly distributed on the volunteer's face 1cm 2 Areas, one of which uses the test side emulsions prepared in Application Examples 1 to 13 and Comparative Application Examples 1 to 6, and the other area uses the blank control side emulsion (the blank control side emulsion, calculated by mass percentage, includes 10% polydimethylsiloxane, 4% squalane, 5% isohexadecane, 3% glycerol, 5% butylene glycol, 3% hyaluronic acid, 5% glyceryl stearate, and the balance is water) as a negative control area.

[0163] Apply once a day for 28 consecutive days, with data collection in two areas on day 0 and day 28 of continuous use. The transepidermal water loss (TEWL) value of skin water loss was tested to reflect the stratum corneum barrier function of the subjects and evaluate the moisturizing efficacy of different groups of lotions.

[0164] Relative transepidermal water loss rate on the 28th day = (T28-T0) / T0×100%.

[0165] Among them, T0 is the transepidermal water loss rate on day 0, and T28 is the transepidermal water loss rate on day 28.

[0166] Table 4

[0167]

[0168]

[0169] Test Example 4

[0170] Irritation test

[0171] According to the relevant requirements and determination methods of the "Human Skin Patch Test" in the "Cosmetic Hygiene Standards", the emulsions prepared in Application Examples 1 to 3 of the present invention and Comparative Application Examples 1 to 3 were tested for safety, and the skin reactions were observed at 0.5 h, 24 h, and 48 h, respectively. The results are shown in Table 5. The test results of all subjects were negative, and no adverse skin reactions occurred.

[0172] Table 5

[0173]

[0174]

[0175] Based on the test data in Tables 2 to 5, it can be seen from the comparison of the data of Example 1 / Application Example 1 and Comparative Examples 1 to 6 / Comparative Application Examples 1 to 6 that when the raw materials for preparing the anti-aging composition lack any component of Dendrobium officinale, Camellia japonica or Polygonatum sibiricum, the promoting effect of the composition on COL-1 secretion and the inhibiting effect on MMP-1 secretion are greatly reduced, and the regulating effect on skin elasticity and the moisturizing effect are also reduced to varying degrees, indicating that Dendrobium officinale, Camellia japonica and Polygonatum sibiricum have a good synergistic effect in promoting COL-1 secretion and inhibiting MMP-1 secretion.

[0176] It can be seen from the data of Example 1 / Application Example 1 and Example 4 / Application Example 4 that in the preparation process of the anti-aging composition, ultra-high pressure treatment of the preparation raw materials before hot reflux extraction can increase the content of active ingredients in the prepared anti-aging composition, promote COL-1 secretion, inhibit MMP-1 secretion, and improve skin elasticity.

[0177] It can be seen from the data of Example 1 / Application Example 1 and Examples 5 to 7 / Application Examples 5 to 7 that in the preparation process of the anti-aging composition, the crude extract is mixed with the composite enzyme for enzymatic hydrolysis reaction. The papain, cellulase and pectinase in the composite enzyme have a certain synergistic effect, which helps to release the active ingredients in the preparation raw materials, thereby improving skin elasticity and moisturizing effects.

[0178] It can be seen from the data of Example 1 / Application Example 1 and Examples 8 to 10 / Application Examples 8 to 10 that after enzymatic hydrolysis, sodium alginate, guar gum and gelatin are used as flocculants to flocculate the enzymatic hydrolysis products, and the three flocculants cooperate with each other to synergistically enhance the effect, thereby obtaining a better flocculation effect, so that the prepared composition can better promote COL-1 secretion, inhibit MMP-1 secretion, and improve the anti-aging effect of the composition.

[0179] It can be seen from the data of Example 1 / Application Example 1 and Examples 11-12 / Application Examples 11-12 that in the preparation process of the anti-aging composition, the use of D101 and DM301 macroporous resins for doping and purification can specifically adsorb and separate a variety of effective ingredients, improve the selectivity and effect of purification, and thereby enable the prepared composition to better improve skin elasticity and moisturizing effects.

[0180] It can be seen from the data of Example 1 / Application Example 1 and Example 13 / Application Example 13 that mixing Dendrobium officinale, Camellia japonica and Polygonatum sibiricum for co-extraction can better exert the anti-aging effect compared to obtaining Dendrobium officinale extract, Camellia japonica extract and Polygonatum sibiricum extract separately and then mixing them.

[0181] It can be seen from the data of Test Example 4 that the anti-aging composition of the present invention has no irritation to the skin and is highly safe.

[0182] The applicant declares that the present invention illustrates the technical solution of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned embodiments, that is, it does not mean that the present invention must rely on the above-mentioned embodiments to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of various raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0183] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0184] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

Claims

1. An anti-aging composition, characterized in that: The raw materials for preparing the anti-aging composition include dendrobium officinale, camellia sinensis and polygonatum cyrtonema.

2. The anti-aging composition according to claim 1, characterized in that In parts by weight, the raw materials for preparing the anti-aging composition include 1 part of Dendrobium officinale, 1-10 parts of Camellia japonica, and 0.5-5 parts of Polygonatum sibiricum.

3. The anti-aging composition according to claim 1 or 2, characterized in that: The anti-aging composition is prepared by a preparation method comprising the following steps: (1) mixing the raw materials for preparing the anti-aging composition with a solvent and performing hot reflux extraction to obtain a crude extract; (2) mixing the crude extract with the composite enzyme to perform an enzymatic hydrolysis reaction to obtain an enzymatic hydrolysis product; (3) The enzymatic hydrolysis product is subjected to flocculation treatment and purification to obtain the anti-aging composition.

4. The anti-aging composition according to claim 3, characterized in that Before the hot reflux extraction in step (1), the step further includes subjecting the prepared raw material to ultra-high pressure treatment; Preferably, the pressure of the ultra-high pressure treatment is 200-350 MPa, and the holding time is 5-15 min.

5. The anti-aging composition according to claim 3 or 4, characterized in that: The number of times of the hot reflux extraction in step (1) is 1 to 4 times, and the time of each hot reflux extraction is 1 to 3 hours; Preferably, the solvent comprises an aqueous solution of ethanol; Preferably, the volume percentage of ethanol in the ethanol aqueous solution is 50-80%.

6. The anti-aging composition according to any one of claims 3 to 5, characterized in that: The complex enzyme in step (2) comprises papain, cellulase and pectinase; Preferably, the mass ratio of papain, cellulase and pectinase is 1:(1-10):(0.5-10); Preferably, the mass ratio of the crude extract to the complex enzyme is (30-100):1; Preferably, the temperature of the enzymatic hydrolysis reaction is 20-50° C., and the time is 0.5-2 h.

7. The anti-aging composition according to any one of claims 3 to 6, characterized in that: The flocculation treatment in step (3) includes mixing the enzymatic hydrolysis product with a flocculant for flocculation treatment; Preferably, the flocculant comprises any one of sodium alginate, guar gum or gelatin, or a combination of at least two thereof; Preferably, the flocculant comprises sodium alginate, guar gum and gelatin; Preferably, the mass ratio of sodium alginate, guar gum and gelatin is 1:(1-5):(1-3); Preferably, the mass of the flocculant is 0.1-2% of the mass of the enzymatic hydrolysis product; Preferably, after the flocculation treatment in step (3), activated carbon is added for decolorization.

8. The anti-aging composition according to any one of claims 3 to 7, characterized in that: The purification in step (3) comprises purifying with a macroporous resin and eluting with water and an aqueous solution of ethanol in sequence, and collecting the aqueous solution of ethanol; Preferably, the type of the macroporous resin includes any one of type D101, type DM301 or type AB-8, or a combination of at least two of them; Preferably, the types of the macroporous resin include D101 and DM301; Preferably, the flow rate of eluting with water is 0.5 to 2 BV / h, and the amount used is 1 to 3 BV; Preferably, the flow rate of elution with ethanol aqueous solution is 0.5 to 2 BV / h, and the amount is 1 to 3 BV; Preferably, when eluting with an ethanol aqueous solution, the volume percentage of ethanol in the ethanol aqueous solution is 50% to 65%.

9. The anti-aging composition according to any one of claims 3 to 8, characterized in that: After the purification in step (3), the step further comprises concentration and drying; Preferably, the concentration comprises concentration under reduced pressure; Preferably, the drying comprises freeze drying or spray drying.

10. Use of the anti-aging composition according to any one of claims 1 to 9 in cosmetics.

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