CN117017855A - Collagen peptide liposome and moisturizing and anti-aging cosmetic - Google Patents
Collagen peptide liposome and moisturizing and anti-aging cosmetic Download PDFInfo
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- CN117017855A CN117017855A CN202310989078.XA CN202310989078A CN117017855A CN 117017855 A CN117017855 A CN 117017855A CN 202310989078 A CN202310989078 A CN 202310989078A CN 117017855 A CN117017855 A CN 117017855A
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- 210000001700 mitochondrial membrane Anatomy 0.000 description 1
- JXTPJDDICSTXJX-UHFFFAOYSA-N n-Triacontane Natural products CCCCCCCCCCCCCCCCCCCCCCCCCCCCCC JXTPJDDICSTXJX-UHFFFAOYSA-N 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000004405 propyl p-hydroxybenzoate Substances 0.000 description 1
- 235000010232 propyl p-hydroxybenzoate Nutrition 0.000 description 1
- QELSKZZBTMNZEB-UHFFFAOYSA-N propylparaben Chemical compound CCCOC(=O)C1=CC=C(O)C=C1 QELSKZZBTMNZEB-UHFFFAOYSA-N 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000037394 skin elasticity Effects 0.000 description 1
- 230000008491 skin homeostasis Effects 0.000 description 1
- 230000036556 skin irritation Effects 0.000 description 1
- 231100000475 skin irritation Toxicity 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- 229940032094 squalane Drugs 0.000 description 1
- 210000000498 stratum granulosum Anatomy 0.000 description 1
- 210000000437 stratum spinosum Anatomy 0.000 description 1
- 210000004003 subcutaneous fat Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229940074410 trehalose Drugs 0.000 description 1
- VLPFTAMPNXLGLX-UHFFFAOYSA-N trioctanoin Chemical compound CCCCCCCC(=O)OCC(OC(=O)CCCCCCC)COC(=O)CCCCCCC VLPFTAMPNXLGLX-UHFFFAOYSA-N 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
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- A61K8/14—Liposomes; Vesicles
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/60—Sugars; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
- A61K8/65—Collagen; Gelatin; Keratin; Derivatives or degradation products thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/78—Connective tissue peptides, e.g. collagen, elastin, laminin, fibronectin, vitronectin or cold insoluble globulin [CIG]
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- C12P21/06—Preparation of peptides or proteins produced by the hydrolysis of a peptide bond, e.g. hydrolysate products
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- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
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- A61K2800/52—Stabilizers
- A61K2800/522—Antioxidants; Radical scavengers
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- A61K2800/74—Biological properties of particular ingredients
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- A61K2800/782—Enzyme inhibitors; Enzyme antagonists
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Abstract
The invention discloses a collagen peptide liposome and a moisturizing and anti-aging cosmetic, wherein the preparation method of the collagen peptide liposome comprises the following steps: extracting collagen from squid skin; preparing collagen peptide; collagen peptide liposomes were prepared. The collagen peptide liposome is prepared and used in the moisturizing and anti-aging cosmetics, and the synergistic flower and leaf extract is added into the moisturizing and anti-aging cosmetics.
Description
Technical Field
The invention relates to the technical field of cosmetics, in particular to collagen peptide liposome and a moisturizing and anti-aging cosmetic.
Background
With the aging, the activities of active substances such as superoxide dismutase, catalase, glutathione reductase and the like which can remove free radicals in human bodies are reduced, and excessive free radicals which are not removed in time react with unsaturated fatty acids such as cell membranes, mitochondrial membranes and the like to form peroxidized lipids, and initiate free radical chain reactions, which are one of the causes of skin aging. In addition, unhealthy lifestyles and neglect of skin care can also accelerate skin aging, leading to premature skin relaxation, loss of elasticity, generation of fine lines, large deposition of pigments, and other problems. There are many types of cosmetics available in the market for preventing and delaying aging, but most of the effects are not ideal.
Chinese patent CN102462640a discloses a marine fish skin collagen moisturizing and anti-aging cosmetic and preparation method thereof, comprising the following steps: soaking and flushing the frozen and preserved fish skin with phosphate buffer solution to remove scales and residual meat, cutting into small pieces, and soaking and flushing with deionized water; soaking in NaOH solution, and cleaning with deionized water; performing restriction enzymolysis, centrifuging, collecting supernatant, and dialyzing; concentrating, freeze drying to obtain marine fish skin collagen; uniformly mixing sodium carboxymethyl cellulose with deionized water, sequentially adding 1, 3-butanediol, sodium hyaluronate, trehalose, vitamin E, marine fish skin collagen, squalane, methyl benzoate and sodium dodecyl sulfonate into deionized water for dissolution, and heating to obtain a solution (1); sequentially adding mineral oil, caprylic triglyceride, alkyl glycoside, jojoba oil and propyl p-hydroxybenzoate, dissolving in a stirrer, heating and stirring to obtain solution (2); mixing, homogenizing, maintaining in water bath, and cooling; the marine fish skin collagen moisturizing and anti-aging cosmetic disclosed by the invention can help the reconstruction of collagen and the regeneration and renewal of elastic collagen in vivo, can block the direct irradiation of ultraviolet rays to skin and delay skin aging, but has poor absorption effect when the marine fish skin collagen is directly used in the cosmetic, and has low utilization rate of active ingredients of the cosmetic.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides collagen peptide liposome and moisturizing and anti-aging cosmetics.
In order to solve the technical problems, the invention adopts the following technical scheme:
the preparation method of the collagen peptide liposome comprises the following steps:
s1, extracting collagen: washing squid skin with water, fishing out, shearing squid Pi Suikuai with the thickness of 5 multiplied by 5mm, putting into a 3-6wt% sodium hydroxide aqueous solution, stirring and leaching at the room temperature at the rotating speed of 150-300rpm for 20-30h, wherein the mass ratio of squid skin fragments to the 3-6wt% sodium hydroxide aqueous solution is 1: (8-12), taking out, washing with water to be neutral, and obtaining alkali-treated squid skin; then putting the alkali-treated squid skin into 0.5-2wt% of tartaric acid aqueous solution, stirring and leaching for 15-20h at the temperature of 42-55 ℃ and the rotating speed of 400-600rpm, wherein the mass ratio of the alkali-treated squid skin to the 0.5-2wt% of tartaric acid aqueous solution is 1: (8-12), centrifuging at 4000-5000rpm for 15-25min, and freeze-drying supernatant to obtain collagen;
s2, preparation of collagen peptide: adding 8-15 parts by weight of collagen obtained by S1 into 25-35 parts by weight of 0.1-0.3mol/L phosphate buffer solution to obtain collagen liquid, and then adding 0.3-0.8 part by weight of hydrolase to perform enzymolysis reaction, wherein the enzymolysis reaction conditions are as follows: inactivating enzyme at 100deg.C for 4-6min at 40-52deg.C and pH 7-8 for 4-6 hr, cooling the enzymolysis solution to room temperature, centrifuging at 1500-3000rpm for 5-10min, and lyophilizing the supernatant to obtain collagen peptide;
S3, preparing collagen peptide liposome: adding 1-3 parts by weight of L-alpha-phosphatidylcholine and 0.4-1 part by weight of the collagen peptide obtained by S2 into a round-bottomed flask filled with 15-25 parts by weight of absolute ethyl alcohol, rotationally evaporating for 30-50min at a rotating speed of 90-110rpm under the water bath condition of 35-45 ℃ by using a rotary evaporator, drying for 15-30min in a vacuum drying oven of 35-50 ℃, taking out a lipid film in the flask, adding 15-25 parts by weight of water, stirring for 10-20min at a rotating speed of 500-700rpm, and then treating for 10-20min in an ultrasonic pulverizer with an ultrasonic frequency of 15-25kHz and an amplitude of 20-35% at 0 ℃ to obtain the collagen peptide liposome.
Human skin consists of three layers, epidermis, dermis and subcutaneous fat, where the epidermis itself consists of four sublayers, namely the basal layer, the stratum spinosum, the stratum granulosum, the stratum hyaline and the outermost stratum corneum. The stratum corneum, which is composed of layers of intracellular lipid components and keratinocytes, plays an important role in forming a skin barrier that protects the body from external threats.
Collagen is a major structural protein constituting connective tissue extracellular matrix, and has weak antigenicity and good biocompatibility. The absorption rate of collagen peptides is affected by the disturbance of the stratum corneum as a skin barrier. In order to improve the utilization rate of the collagen, the collagen peptide is hydrolyzed under certain conditions to generate the collagen peptide, compared with the collagen, the collagen peptide has the advantages of increased polar groups and further enhanced solubility, obviously increased water absorption and water holding capacity, and has a plurality of biological activities besides the general functional characteristics of the protein, such as antioxidant activity, antimicrobial activity and beneficial effects on skin, bones or joint health. Compared with high molecular weight natural collagen, small molecular weight collagen peptide penetrates deep into skin more easily through stratum corneum, and can play important roles in growth of fibroblast, collagen expression and formation of strong collagen fibers in epidermis, and can maintain skin homeostasis and repair damaged skin layers by increasing water content of stratum corneum. In order to maximally improve the skin permeability of the collagen peptide, the elastic nanoliposome is used as a carrier of the collagen peptide, and has elasticity and flexibility compared with the traditional nanoliposome.
Preferably, the preparation method of the collagen peptide liposome comprises the following steps:
s1, extracting collagen: washing squid skin with water, fishing out, shearing squid Pi Suikuai with the thickness of 5 multiplied by 5mm, putting into a 3-6wt% sodium hydroxide aqueous solution, stirring and leaching at the room temperature at the rotating speed of 150-300rpm for 20-30h, wherein the mass ratio of squid skin fragments to the 3-6wt% sodium hydroxide aqueous solution is 1: (8-12), taking out, washing with water to be neutral, and obtaining alkali-treated squid skin; then putting the alkali-treated squid skin into 0.5-2wt% of tartaric acid aqueous solution, stirring and leaching for 15-20h at the temperature of 42-55 ℃ and the rotating speed of 400-600rpm, wherein the mass ratio of the alkali-treated squid skin to the 0.5-2wt% of tartaric acid aqueous solution is 1: (8-12), centrifuging at 4000-5000rpm for 15-25min, and freeze-drying supernatant to obtain crude collagen; and finally, adding the crude collagen into ice water at 0 ℃, wherein the mass ratio of the crude collagen to the ice water at 0 ℃ is 1: (8-12), placing the mixture into an ultrasonic wave with the ultrasonic frequency of 35-40kHz and the ultrasonic power of 300-400W for ultrasonic extraction for 40-80min, centrifuging at 3500-4500rpm for 15-30min after the ultrasonic extraction is finished, and taking supernatant for freeze drying to obtain collagen;
s2, preparation of collagen peptide: adding 8-15 parts by weight of collagen obtained by S1 into 25-35 parts by weight of 0.1-0.3mol/L phosphate buffer solution to obtain collagen liquid, and then adding 0.3-0.8 part by weight of hydrolase to perform enzymolysis reaction, wherein the enzymolysis reaction conditions are as follows: inactivating enzyme at 100deg.C for 4-6min at 40-52deg.C and pH 7-8 for 4-6 hr, cooling the enzymolysis solution to room temperature, centrifuging at 1500-3000rpm for 5-10min, and lyophilizing the supernatant to obtain collagen peptide;
S3, preparing collagen peptide liposome: adding 1-3 parts by weight of L-alpha-phosphatidylcholine and 0.4-1 part by weight of the collagen peptide obtained by S2 into a round-bottomed flask filled with 15-25 parts by weight of absolute ethyl alcohol, rotationally evaporating for 30-50min at a rotating speed of 90-110rpm under the water bath condition of 35-45 ℃ by using a rotary evaporator, drying for 15-30min in a vacuum drying oven of 35-50 ℃, taking out a lipid film in the flask, adding 15-25 parts by weight of water, stirring for 10-20min at a rotating speed of 500-700rpm, and then treating for 10-20min in an ultrasonic pulverizer with an ultrasonic frequency of 15-25kHz and an amplitude of 20-35% at 0 ℃ to obtain the collagen peptide liposome.
The crude collagen is further extracted by utilizing ultrasonic, and mainly because the crude collagen contains undamaged whole cell tissues, the collagen in the crude collagen cannot be released, cell membranes can be effectively damaged by utilizing ultrasonic vibration to release cell contents, and the cell tissue structure is highly loosened due to repeated cavitation and impact caused by ultrasonic, so that the collagen can be better released after strong homogenization, and the extraction rate of the collagen can be further improved.
Further preferably, the preparation method of the collagen peptide liposome comprises the following steps:
S1, extracting collagen: washing squid skin with water, fishing out, shearing squid Pi Suikuai with the thickness of 5 multiplied by 5mm, putting into a 3-6wt% sodium hydroxide aqueous solution, stirring and leaching at the room temperature at the rotating speed of 150-300rpm for 20-30h, wherein the mass ratio of squid skin fragments to the 3-6wt% sodium hydroxide aqueous solution is 1: (8-12), taking out, washing with water to be neutral, and obtaining alkali-treated squid skin; then putting the alkali-treated squid skin into 0.5-2wt% of tartaric acid aqueous solution, stirring and leaching for 15-20h at the temperature of 42-55 ℃ and the rotating speed of 400-600rpm, wherein the mass ratio of the alkali-treated squid skin to the 0.5-2wt% of tartaric acid aqueous solution is 1: (8-12), centrifuging at 4000-5000rpm for 15-25min, and freeze-drying supernatant to obtain crude collagen; and finally, adding the crude collagen into ice water at 0 ℃, wherein the mass ratio of the crude collagen to the ice water at 0 ℃ is 1: (8-12), placing the mixture into an ultrasonic wave with the ultrasonic frequency of 35-40kHz and the ultrasonic power of 300-400W for ultrasonic extraction for 40-80min, centrifuging at 3500-4500rpm for 15-30min after the ultrasonic extraction is finished, and taking supernatant for freeze drying to obtain collagen;
s2, preparation of collagen peptide: adding 8-15 parts by weight of collagen obtained by S1 into 25-35 parts by weight of 0.1-0.3mol/L phosphate buffer solution to obtain collagen liquid, and then adding 0.3-0.8 part by weight of hydrolase to perform enzymolysis reaction, wherein the enzymolysis reaction conditions are as follows: inactivating enzyme at 100deg.C for 4-6min at 40-52deg.C and pH 7-8 for 4-6 hr, cooling the enzymolysis solution to room temperature, centrifuging at 1500-3000rpm for 5-10min, and lyophilizing the supernatant to obtain collagen peptide;
S3, preparing collagen peptide liposome: adding 1-3 parts by weight of L-alpha-phosphatidylcholine, 0.2-0.7 parts by weight of edge activator and 0.4-1 part by weight of collagen peptide obtained by S2 into a round bottom flask containing 15-25 parts by weight of absolute ethyl alcohol, rotationally evaporating at a rotating speed of 90-110rpm for 30-50min under the water bath condition of 35-45 ℃ by using a rotary evaporator, drying for 15-30min in a vacuum drying oven of 35-50 ℃, taking out a lipid film in the flask, adding 15-25 parts by weight of water, stirring for 10-20min at the rotating speed of 500-700rpm, and then treating for 10-20min in an ultrasonic pulverizer with the ultrasonic frequency of 15-25kHz and the amplitude of 20-35% at 0 ℃ to obtain collagen peptide liposome.
The hydrolase is one or more of papain, trypsin, aspergillus niger acid protease, pepsin and subtilisin; preferably, the hydrolase is a mixture of trypsin and subtilisin, wherein the mass ratio of trypsin to subtilisin is (1-3): 1.
the hydrolyzed amino acid residue site of trypsin is carboxyl terminal peptide bond of glutamic acid, methionine, lysine or glutamine; whereas subtilisin has a strong specificity for the carboxy-terminal hydrophobic amino acids, it recognizes and cleaves the carboxy-terminal peptide bond of aromatic or hydrophobic amino acids such as tyrosine, phenylalanine, tryptophan or leucine. Therefore, the trypsin and the subtilisin are simultaneously used as the hydrolytic enzymes of the collagen, so that the collagen can be more thoroughly hydrolyzed, the yield of the collagen peptide is improved, more short peptide chains with low molecular weight and free amino acid residues can be obtained, and the antioxidant capacity of the collagen peptide is improved.
The edge activator is one of Tween 80, sodium cetyl sulfate, cholesterol and sucrose distearate; preferably, the edge activator is sucrose distearate.
According to the invention, the edge activator-sucrose distearate is added in the preparation process of the nano liposome, so that the oxidation speed of the liposome can be slowed down, the liposome is promoted to be stable, and meanwhile, the liposome can be filled between the bilayer of the liposome, so that the fluidity of the bilayer is regulated, and the encapsulation efficiency of the collagen peptide is effectively improved. Sucrose distearate is a nonionic surfactant, also a natural sugar derived ingredient, and has various functions in the cosmetic, pharmaceutical and food industries, and it can also improve the moisturizing property and emulsion stability of nanoliposomes in the present invention. Compared with an edge activator with a single alkyl chain, the sucrose distearate has two long alkyl chains, so that on one hand, electrostatic repulsive force generated among prepared liposome particles is increased, thereby increasing the surface charge of the liposome, increasing the resistance which needs to be overcome when the liposome is aggregated, and further increasing the stability of the liposome; on the other hand, the method can effectively reduce the melting point of the elastic nanoliposome, weaken the crystallinity of the nanoliposome, increase the membrane fluidity of the nanoliposome, further increase the deformability of the elastic nanoliposome, and be beneficial to the nanoliposome to effectively penetrate the stratum corneum of the skin, so that the active ingredient-collagen peptide is conveyed into the skin deeper.
A moisturizing and antiaging cosmetic comprises the collagen peptide liposome.
A moisturizing and anti-aging cosmetic comprises the following raw materials in parts by weight: 4-6 parts by weight of ethylhexyl palmitate, 1-3 parts by weight of cyclopentasiloxane, 1.5-2.5 parts by weight of C12-15 alcohol benzoate, 0.4-0.8 part by weight of carbomer 940, 1.5-2.4 parts by weight of betaine, 0.3-0.7 part by weight of emulsifier, 0.2-0.5 part by weight of sodium hyaluronate, 0.1-0.3 part by weight of arginine, 0.2-0.5 part by weight of allantoin, 3-6 parts by weight of collagen peptide liposome and 90-105 parts by weight of water.
Preferably, the moisturizing and anti-aging cosmetic further comprises 0.4-0.8 part by weight of synergistic flower and leaf extract.
The preparation method of the synergistic flower and leaf extract comprises the following steps:
taking dried Du Lianhua and perilla leaves, crushing, sieving with a 50-80 mesh sieve, uniformly mixing according to a mass ratio of 3 (1-2), obtaining a standby raw material, then putting into an ethanol water solution with a weight ratio of 82-88wt%, wherein the mass ratio of the standby raw material to the ethanol water solution is 1 (7-10), stirring and leaching at a rotating speed of 200-300rpm for 2-3h at 55-65 ℃, then placing into ultrasonic waves with an ultrasonic frequency of 30-40kHz and an ultrasonic power of 300-500W for 1-2h, filtering, collecting filtrate, concentrating under reduced pressure, and removing an organic solvent to obtain a crude extract;
A2, adopting macroporous adsorption resin to adsorb and purify the crude extract, and then washing to remove impurities, wherein the flow rate is 2-3BV/h; eluting with 40-50wt% ethanol water solution at flow rate of 2-3BV/h, collecting eluate, concentrating under reduced pressure to remove organic solvent, and freeze drying to obtain synergistic flower and leaf extract.
The emulsifier is any one of tridecyl alcohol ether-6, glyceryl monostearate, polyoxyethylene stearate and sorbitan stearate 165.
The invention also provides a preparation method of the moisturizing and anti-aging cosmetic, which comprises the following steps:
(1) Uniformly mixing ethylhexyl palmitate, cyclopentasiloxane and C12-15 alcohol benzoate, and heating to 75-85 ℃ to obtain a phase A; adding carbomer 940, betaine, emulsifier, sodium hyaluronate, arginine, allantoin, and synergistic folium Phyllostachydis Henonis extract into water, mixing, and heating to 75-85deg.C to obtain phase B;
(2) And stirring the phase B at 500-1000rpm for 8-12min, adding the phase A, stirring for 25-40min, adding collagen peptide liposome, and stirring for 15-30min to obtain the moisturizing and anti-aging cosmetic.
The invention has the beneficial effects that: the collagen peptide liposome prepared by the invention is used in moisturizing and anti-aging cosmetics, and has good moisturizing effect, anti-aging effect and whitening effect. One of the active ingredients, namely collagen peptide liposome, contains sucrose distearate with moisturizing effect, and can reduce water dispersion on the surface layer of skin, keep the skin moist and reduce fine wrinkles; on the other hand, the collagen peptide in the collagen liposome can be preferentially combined with fatty acid free radicals to stop the free radical chain reaction, so that lipid peroxidation is inhibited, free radical generation is reduced, meanwhile, the collagen peptide can also effectively remove excessive active oxygen free radicals in the body, protect normal structures and functions of cells and mitochondria, promote the increase of collagen fiber content in the skin, promote the enhancement of skin elasticity and compliance, and achieve the anti-aging purpose; in addition, the collagen peptide in the collagen liposome can effectively chelate Cu 2+ The combination of tyrosine and tyrosinase catalytic active center is hindered, and the oxidation function of tyrosinase is directly inhibited, so that the tyrosinase is inhibited, the melanin content is reduced, and the whitening effect is achieved.
Detailed Description
The above summary of the present application is described in further detail below in conjunction with the detailed description, but it should not be understood that the scope of the above-described subject matter of the present application is limited to the following examples.
Introduction of partial raw materials in the application:
ethylhexyl palmitate, CAS no: 29806-73-3.
Ethylhexyl palmitate has stable chemical properties and no peculiar smell, can lubricate skin without greasy feeling when used in cosmetics, is easy to be absorbed by skin, and is an excellent skin softener.
Decamethylcyclopentasiloxane, CAS No.: 541-02-6.
C12-15 alcohol benzoate, CAS number: 68411-27-8.
Betaine, CAS number: 107-43-7.
Betaine has strong binding effect with polar terminal molecule of hydrogen atom, can be strongly bound with water molecule, and has effects of reducing skin irritation and keeping moisture in cosmetic formulation.
Trideceth-6, cas No.: 24938-91-8.
Tridecyl alcohol ether-6 has extremely strong penetrating, dispersing and emulsifying capacity, and can be used as an emulsifying agent in a cosmetic formula to make the product more stable.
The squid skin is prepared from Peruvian squid skin provided by Zhejiang Kyoho company, and is frozen at-18deg.C after cleaning.
L-alpha-phosphatidylcholine, CAS number: 8002-43-5.
Sucrose distearate, CAS number: 27195-16-0.
Trypsin, enzyme activity: 10U/g, zhengzhou Weifeng Biotechnology Co., ltd.
Subtilisin, enzyme activity: 10U/g, ningxia and the wall biotechnology Co.
H103 macroporous adsorbent resin, cat No. M0075, beijing solebao technologies limited.
Preparation example 1
The preparation method of the collagen peptide liposome comprises the following steps:
s1, extracting collagen: washing squid skin with water, fishing out, shearing squid Pi Suikuai with the thickness of 5 multiplied by 5mm, putting into 5wt% sodium hydroxide aqueous solution, stirring and leaching for 24 hours at room temperature at a rotating speed of 200rpm, wherein the mass ratio of squid skin fragments to the 5wt% sodium hydroxide aqueous solution is 1:10, taking out, washing with water to be neutral to obtain alkali-treated squid skin; then putting the alkali-treated squid skin into 1wt% tartaric acid aqueous solution, stirring and leaching for 18h at the temperature of 50 ℃ and the rotating speed of 500rpm, wherein the mass ratio of the alkali-treated squid skin to the 1wt% tartaric acid aqueous solution is 1:10, centrifuging at 4500rpm for 20min, and freeze-drying supernatant to obtain collagen;
S2, preparation of collagen peptide: adding 10 parts by weight of the collagen obtained in the step S1 into 30 parts by weight of 0.2mol/L phosphate buffer solution to obtain collagen liquid, and then adding 0.5 part by weight of hydrolase to perform enzymolysis reaction, wherein the enzymolysis reaction conditions are as follows: inactivating enzyme at 100deg.C for 5min after finishing at 50deg.C and pH=7.5 for 5 hr, cooling the enzymolysis solution to room temperature, centrifuging at 2000rpm for 8min, and lyophilizing supernatant to obtain collagen peptide; the hydrolase is trypsin;
s3, preparing collagen peptide liposome: 1.5 parts by weight of L-alpha-phosphatidylcholine and 0.5 part by weight of the collagen peptide obtained by S2 are added into a round-bottomed flask filled with 20 parts by weight of absolute ethyl alcohol, rotary evaporation is carried out for 40min at a rotating speed of 100rpm under the water bath condition of 40 ℃ by using a rotary evaporator, the mixture is dried for 20min in a vacuum drying oven of 40 ℃, the lipid film in the flask is taken out, 20 parts by weight of water is added into the mixture and stirred for 15min at a rotating speed of 600rpm, and then the mixture is treated for 15min in an ultrasonic pulverizer with an ultrasonic frequency of 20kHz and an amplitude of 30% at 0 ℃ to obtain collagen peptide liposome.
Preparation example 2
The preparation method of the collagen peptide liposome comprises the following steps:
S1, extracting collagen: washing squid skin with water, fishing out, shearing squid Pi Suikuai with the thickness of 5 multiplied by 5mm, putting into 5wt% sodium hydroxide aqueous solution, stirring and leaching for 24 hours at room temperature at a rotating speed of 200rpm, wherein the mass ratio of squid skin fragments to the 5wt% sodium hydroxide aqueous solution is 1:10, taking out, washing with water to be neutral to obtain alkali-treated squid skin; then putting the alkali-treated squid skin into 1wt% tartaric acid aqueous solution, stirring and leaching for 18h at the temperature of 50 ℃ and the rotating speed of 500rpm, wherein the mass ratio of the alkali-treated squid skin to the 1wt% tartaric acid aqueous solution is 1:10, centrifuging at 4500rpm for 20min, and freeze-drying supernatant to obtain crude collagen; and finally, adding the crude collagen into ice water at 0 ℃, wherein the mass ratio of the crude collagen to the ice water at 0 ℃ is 1:10, performing ultrasonic extraction for 60min at ultrasonic frequency of 38kHz and ultrasonic power of 350W, centrifuging at 4000rpm for 20min after the ultrasonic extraction is finished, and freeze-drying supernatant to obtain collagen;
s2, preparation of collagen peptide: adding 10 parts by weight of the collagen obtained in the step S1 into 30 parts by weight of 0.2mol/L phosphate buffer solution to obtain collagen liquid, and then adding 0.5 part by weight of hydrolase to perform enzymolysis reaction, wherein the enzymolysis reaction conditions are as follows: inactivating enzyme at 100deg.C for 5min after finishing at 50deg.C and pH=7.5 for 5 hr, cooling the enzymolysis solution to room temperature, centrifuging at 2000rpm for 8min, and lyophilizing supernatant to obtain collagen peptide; the hydrolase is trypsin;
S3, preparing collagen peptide liposome: 1.5 parts by weight of L-alpha-phosphatidylcholine and 0.5 part by weight of the collagen peptide obtained by S2 are added into a round-bottomed flask filled with 20 parts by weight of absolute ethyl alcohol, rotary evaporation is carried out for 40min at a rotating speed of 100rpm under the water bath condition of 40 ℃ by using a rotary evaporator, the mixture is dried for 20min in a vacuum drying oven of 40 ℃, the lipid film in the flask is taken out, 20 parts by weight of water is added into the mixture and stirred for 15min at a rotating speed of 600rpm, and then the mixture is treated for 15min in an ultrasonic pulverizer with an ultrasonic frequency of 20kHz and an amplitude of 30% at 0 ℃ to obtain collagen peptide liposome.
Preparation example 3
The preparation method of the collagen peptide liposome comprises the following steps:
s1, extracting collagen: washing squid skin with water, fishing out, shearing squid Pi Suikuai with the thickness of 5 multiplied by 5mm, putting into 5wt% sodium hydroxide aqueous solution, stirring and leaching for 24 hours at room temperature at a rotating speed of 200rpm, wherein the mass ratio of squid skin fragments to the 5wt% sodium hydroxide aqueous solution is 1:10, taking out, washing with water to be neutral to obtain alkali-treated squid skin; then putting the alkali-treated squid skin into 1wt% tartaric acid aqueous solution, stirring and leaching for 18h at the temperature of 50 ℃ and the rotating speed of 500rpm, wherein the mass ratio of the alkali-treated squid skin to the 1wt% tartaric acid aqueous solution is 1:10, centrifuging at 4500rpm for 20min, and freeze-drying supernatant to obtain crude collagen; and finally, adding the crude collagen into ice water at 0 ℃, wherein the mass ratio of the crude collagen to the ice water at 0 ℃ is 1:10, performing ultrasonic extraction for 60min at ultrasonic frequency of 38kHz and ultrasonic power of 350W, centrifuging at 4000rpm for 20min after the ultrasonic extraction is finished, and freeze-drying supernatant to obtain collagen;
S2, preparation of collagen peptide: adding 10 parts by weight of the collagen obtained in the step S1 into 30 parts by weight of 0.2mol/L phosphate buffer solution to obtain collagen liquid, and then adding 0.5 part by weight of hydrolase to perform enzymolysis reaction, wherein the enzymolysis reaction conditions are as follows: inactivating enzyme at 100deg.C for 5min after finishing at 50deg.C and pH=7.5 for 5 hr, cooling the enzymolysis solution to room temperature, centrifuging at 2000rpm for 8min, and lyophilizing supernatant to obtain collagen peptide; the hydrolase is trypsin;
s3, preparing collagen peptide liposome: 1.5 parts by weight of L-alpha-phosphatidylcholine, 0.4 part by weight of sucrose distearate and 0.5 part by weight of the collagen peptide obtained by S2 are added into a round-bottomed flask filled with 20 parts by weight of absolute ethyl alcohol, rotary evaporation is carried out for 40min at a rotating speed of 100rpm under the water bath condition of 40 ℃ by using a rotary evaporator, the mixture is placed into a vacuum drying oven of 40 ℃ for drying for 20min, a lipid film in the flask is taken out, 20 parts by weight of water is added and stirred for 15min at a rotating speed of 600rpm, and then the mixture is placed into an ultrasonic pulverizer of which the ultrasonic frequency is 20kHz and the amplitude is 30% at 0 ℃ for processing for 15min, so that the collagen peptide liposome is obtained.
Preparation example 4
The preparation method of the collagen peptide liposome comprises the following steps:
S1, extracting collagen: washing squid skin with water, fishing out, shearing squid Pi Suikuai with the thickness of 5 multiplied by 5mm, putting into 5wt% sodium hydroxide aqueous solution, stirring and leaching for 24 hours at room temperature at a rotating speed of 200rpm, wherein the mass ratio of squid skin fragments to the 5wt% sodium hydroxide aqueous solution is 1:10, taking out, washing with water to be neutral to obtain alkali-treated squid skin; then putting the alkali-treated squid skin into 1wt% tartaric acid aqueous solution, stirring and leaching for 18h at the temperature of 50 ℃ and the rotating speed of 500rpm, wherein the mass ratio of the alkali-treated squid skin to the 1wt% tartaric acid aqueous solution is 1:10, centrifuging at 4500rpm for 20min, and freeze-drying supernatant to obtain crude collagen; and finally, adding the crude collagen into ice water at 0 ℃, wherein the mass ratio of the crude collagen to the ice water at 0 ℃ is 1:10, performing ultrasonic extraction for 60min at ultrasonic frequency of 38kHz and ultrasonic power of 350W, centrifuging at 4000rpm for 20min after the ultrasonic extraction is finished, and freeze-drying supernatant to obtain collagen;
s2, preparation of collagen peptide: adding 10 parts by weight of the collagen obtained in the step S1 into 30 parts by weight of 0.2mol/L phosphate buffer solution to obtain collagen liquid, and then adding 0.5 part by weight of hydrolase to perform enzymolysis reaction, wherein the enzymolysis reaction conditions are as follows: inactivating enzyme at 100deg.C for 5min after finishing at 50deg.C and pH=7.5 for 5 hr, cooling the enzymolysis solution to room temperature, centrifuging at 2000rpm for 8min, and lyophilizing supernatant to obtain collagen peptide; the hydrolase is subtilisin;
S3, preparing collagen peptide liposome: 1.5 parts by weight of L-alpha-phosphatidylcholine, 0.4 part by weight of sucrose distearate and 0.5 part by weight of the collagen peptide obtained by S2 are added into a round-bottomed flask filled with 20 parts by weight of absolute ethyl alcohol, rotary evaporation is carried out for 40min at a rotating speed of 100rpm under the water bath condition of 40 ℃ by using a rotary evaporator, the mixture is placed into a vacuum drying oven of 40 ℃ for drying for 20min, a lipid film in the flask is taken out, 20 parts by weight of water is added and stirred for 15min at a rotating speed of 600rpm, and then the mixture is placed into an ultrasonic pulverizer of which the ultrasonic frequency is 20kHz and the amplitude is 30% at 0 ℃ for processing for 15min, so that the collagen peptide liposome is obtained.
Preparation example 5
The preparation method of the collagen peptide liposome comprises the following steps:
s1, extracting collagen: washing squid skin with water, fishing out, shearing squid Pi Suikuai with the thickness of 5 multiplied by 5mm, putting into 5wt% sodium hydroxide aqueous solution, stirring and leaching for 24 hours at room temperature at a rotating speed of 200rpm, wherein the mass ratio of squid skin fragments to the 5wt% sodium hydroxide aqueous solution is 1:10, taking out, washing with water to be neutral to obtain alkali-treated squid skin; then putting the alkali-treated squid skin into 1wt% tartaric acid aqueous solution, stirring and leaching for 18h at the temperature of 50 ℃ and the rotating speed of 500rpm, wherein the mass ratio of the alkali-treated squid skin to the 1wt% tartaric acid aqueous solution is 1:10, centrifuging at 4500rpm for 20min, and freeze-drying supernatant to obtain crude collagen; and finally, adding the crude collagen into ice water at 0 ℃, wherein the mass ratio of the crude collagen to the ice water at 0 ℃ is 1:10, performing ultrasonic extraction for 60min at ultrasonic frequency of 38kHz and ultrasonic power of 350W, centrifuging at 4000rpm for 20min after the ultrasonic extraction is finished, and freeze-drying supernatant to obtain collagen;
S2, preparation of collagen peptide: adding 10 parts by weight of the collagen obtained in the step S1 into 30 parts by weight of 0.2mol/L phosphate buffer solution to obtain collagen liquid, and then adding 0.5 part by weight of hydrolase to perform enzymolysis reaction, wherein the enzymolysis reaction conditions are as follows: inactivating enzyme at 100deg.C for 5min after finishing at 50deg.C and pH=7.5 for 5 hr, cooling the enzymolysis solution to room temperature, centrifuging at 2000rpm for 8min, and lyophilizing supernatant to obtain collagen peptide; the hydrolase is a mixture of trypsin and subtilisin, wherein the mass ratio of trypsin to subtilisin is 2:1, a step of;
s3, preparing collagen peptide liposome: 1.5 parts by weight of L-alpha-phosphatidylcholine, 0.4 part by weight of sucrose distearate and 0.5 part by weight of the collagen peptide obtained by S2 are added into a round-bottomed flask filled with 20 parts by weight of absolute ethyl alcohol, rotary evaporation is carried out for 40min at a rotating speed of 100rpm under the water bath condition of 40 ℃ by using a rotary evaporator, the mixture is placed into a vacuum drying oven of 40 ℃ for drying for 20min, a lipid film in the flask is taken out, 20 parts by weight of water is added and stirred for 15min at a rotating speed of 600rpm, and then the mixture is placed into an ultrasonic pulverizer of which the ultrasonic frequency is 20kHz and the amplitude is 30% at 0 ℃ for processing for 15min, so that the collagen peptide liposome is obtained.
Preparation example 6
The preparation method of the collagen peptide comprises the following steps:
s1, extracting collagen: washing squid skin with water, fishing out, shearing squid Pi Suikuai with the thickness of 5 multiplied by 5mm, putting into 5wt% sodium hydroxide aqueous solution, stirring and leaching for 24 hours at room temperature at a rotating speed of 200rpm, wherein the mass ratio of squid skin fragments to the 5wt% sodium hydroxide aqueous solution is 1:10, taking out, washing with water to be neutral to obtain alkali-treated squid skin; then putting the alkali-treated squid skin into 1wt% tartaric acid aqueous solution, stirring and leaching for 18h at the temperature of 50 ℃ and the rotating speed of 500rpm, wherein the mass ratio of the alkali-treated squid skin to the 1wt% tartaric acid aqueous solution is 1:10, centrifuging at 4500rpm for 20min, and freeze-drying supernatant to obtain collagen;
s2, preparation of collagen peptide: adding 10 parts by weight of the collagen obtained in the step S1 into 30 parts by weight of 0.2mol/L phosphate buffer solution to obtain collagen liquid, and then adding 0.5 part by weight of hydrolase to perform enzymolysis reaction, wherein the enzymolysis reaction conditions are as follows: inactivating enzyme at 100deg.C for 5min after finishing at 50deg.C and pH=7.5 for 5 hr, cooling the enzymolysis solution to room temperature, centrifuging at 2000rpm for 8min, and lyophilizing supernatant to obtain collagen peptide; the hydrolase is trypsin.
Example 1
A moisturizing and anti-aging cosmetic comprises the following raw materials in parts by weight: 5 parts by weight of ethylhexyl palmitate, 2 parts by weight of cyclopentasiloxane, 2 parts by weight of C12-15 alcohol benzoate, 0.6 part by weight of carbomer 940, 2 parts by weight of betaine, 0.5 part by weight of tridecyl alcohol ether-6, 0.4 part by weight of sodium hyaluronate, 0.2 part by weight of arginine, 0.3 part by weight of allantoin, 4 parts by weight of the collagen peptide liposome of preparation example 1, and 100 parts by weight of water.
The preparation method of the moisturizing and anti-aging cosmetic comprises the following steps:
(1) Uniformly mixing ethylhexyl palmitate, cyclopentasiloxane and C12-15 alcohol benzoate, and heating to 80 ℃ to obtain a phase A; adding carbomer 940, betaine, tridecyl alcohol ether-6, sodium hyaluronate, arginine, and allantoin into water, mixing, and heating to 80deg.C to obtain phase B;
(2) And stirring the phase B at 800rpm for 10min, adding the phase A, continuously stirring for 30min, and continuously stirring for 20min to obtain the moisturizing and anti-aging cosmetic.
Example 2
A moisturizing and anti-aging cosmetic comprises the following raw materials in parts by weight: 5 parts by weight of ethylhexyl palmitate, 2 parts by weight of cyclopentasiloxane, 2 parts by weight of C12-15 alcohol benzoate, 0.6 part by weight of carbomer 940, 2 parts by weight of betaine, 0.5 part by weight of tridecyl alcohol ether-6, 0.4 part by weight of sodium hyaluronate, 0.2 part by weight of arginine, 0.3 part by weight of allantoin, 4 parts by weight of the collagen peptide liposome of preparation example 2, and 100 parts by weight of water.
The preparation method of the moisturizing and anti-aging cosmetic comprises the following steps:
(1) Uniformly mixing ethylhexyl palmitate, cyclopentasiloxane and C12-15 alcohol benzoate, and heating to 80 ℃ to obtain a phase A; adding carbomer 940, betaine, tridecyl alcohol ether-6, sodium hyaluronate, arginine, and allantoin into water, mixing, and heating to 80deg.C to obtain phase B;
(2) And stirring the phase B at 800rpm for 10min, adding the phase A, continuously stirring for 30min, and continuously stirring for 20min to obtain the moisturizing and anti-aging cosmetic.
Example 3
A moisturizing and anti-aging cosmetic comprises the following raw materials in parts by weight: 5 parts by weight of ethylhexyl palmitate, 2 parts by weight of cyclopentasiloxane, 2 parts by weight of C12-15 alcohol benzoate, 0.6 part by weight of carbomer 940, 2 parts by weight of betaine, 0.5 part by weight of tridecyl alcohol ether-6, 0.4 part by weight of sodium hyaluronate, 0.2 part by weight of arginine, 0.3 part by weight of allantoin, 4 parts by weight of the collagen peptide liposome of preparation example 3, and 100 parts by weight of water.
The preparation method of the moisturizing and anti-aging cosmetic comprises the following steps:
(1) Uniformly mixing ethylhexyl palmitate, cyclopentasiloxane and C12-15 alcohol benzoate, and heating to 80 ℃ to obtain a phase A; adding carbomer 940, betaine, tridecyl alcohol ether-6, sodium hyaluronate, arginine, and allantoin into water, mixing, and heating to 80deg.C to obtain phase B;
(2) And stirring the phase B at 800rpm for 10min, adding the phase A, continuously stirring for 30min, and continuously stirring for 20min to obtain the moisturizing and anti-aging cosmetic.
Example 4
A moisturizing and anti-aging cosmetic comprises the following raw materials in parts by weight: 5 parts by weight of ethylhexyl palmitate, 2 parts by weight of cyclopentasiloxane, 2 parts by weight of C12-15 alcohol benzoate, 0.6 part by weight of carbomer 940, 2 parts by weight of betaine, 0.5 part by weight of tridecyl alcohol ether-6, 0.4 part by weight of sodium hyaluronate, 0.2 part by weight of arginine, 0.3 part by weight of allantoin, 4 parts by weight of the collagen peptide liposome of preparation example 4, and 100 parts by weight of water.
The preparation method of the moisturizing and anti-aging cosmetic comprises the following steps:
(1) Uniformly mixing ethylhexyl palmitate, cyclopentasiloxane and C12-15 alcohol benzoate, and heating to 80 ℃ to obtain a phase A; adding carbomer 940, betaine, tridecyl alcohol ether-6, sodium hyaluronate, arginine, and allantoin into water, mixing, and heating to 80deg.C to obtain phase B;
(2) And stirring the phase B at 800rpm for 10min, adding the phase A, continuously stirring for 30min, and continuously stirring for 20min to obtain the moisturizing and anti-aging cosmetic.
Example 5
A moisturizing and anti-aging cosmetic comprises the following raw materials in parts by weight: 5 parts by weight of ethylhexyl palmitate, 2 parts by weight of cyclopentasiloxane, 2 parts by weight of C12-15 alcohol benzoate, 0.6 part by weight of carbomer 940, 2 parts by weight of betaine, 0.5 part by weight of tridecyl alcohol ether-6, 0.4 part by weight of sodium hyaluronate, 0.2 part by weight of arginine, 0.3 part by weight of allantoin, 4 parts by weight of the collagen peptide liposome of preparation example 5, and 100 parts by weight of water.
The preparation method of the moisturizing and anti-aging cosmetic comprises the following steps:
(1) Uniformly mixing ethylhexyl palmitate, cyclopentasiloxane and C12-15 alcohol benzoate, and heating to 80 ℃ to obtain a phase A; adding carbomer 940, betaine, tridecyl alcohol ether-6, sodium hyaluronate, arginine, and allantoin into water, mixing, and heating to 80deg.C to obtain phase B;
(2) And stirring the phase B at 800rpm for 10min, adding the phase A, continuously stirring for 30min, and continuously stirring for 20min to obtain the moisturizing and anti-aging cosmetic.
Example 6
A moisturizing and anti-aging cosmetic comprises the following raw materials in parts by weight: 5 parts by weight of ethylhexyl palmitate, 2 parts by weight of cyclopentasiloxane, 2 parts by weight of C12-15 alcohol benzoate, 0.6 part by weight of carbomer 940, 2 parts by weight of betaine, 0.5 part by weight of tridecanol ether-6, 0.4 part by weight of sodium hyaluronate, 0.2 part by weight of arginine, 0.3 part by weight of allantoin, 1 part by weight of the collagen peptide of preparation 6, 3 parts by weight of L-alpha-phosphatidylcholine, and 100 parts by weight of water.
The preparation method of the moisturizing and anti-aging cosmetic comprises the following steps:
(1) Uniformly mixing ethylhexyl palmitate, cyclopentasiloxane and C12-15 alcohol benzoate, and heating to 80 ℃ to obtain a phase A; adding carbomer 940, betaine, tridecyl alcohol ether-6, sodium hyaluronate, arginine, and allantoin into water, mixing, and heating to 80deg.C to obtain phase B;
(2) Then stirring the phase B at 800rpm for 10min, adding the phase A, stirring for 30min, adding the collagen peptide of preparation 6 and L-alpha-phosphatidylcholine, and stirring for 20min to obtain the moisturizing and anti-aging cosmetic.
Example 7
A moisturizing and anti-aging cosmetic comprises the following raw materials in parts by weight: 5 parts by weight of ethylhexyl palmitate, 2 parts by weight of cyclopentasiloxane, 2 parts by weight of C12-15 alcohol benzoate, 0.6 part by weight of carbomer 940, 2 parts by weight of betaine, 0.5 part by weight of tridecyl alcohol ether-6, 0.4 part by weight of sodium hyaluronate, 0.2 part by weight of arginine, 0.3 part by weight of allantoin, 0.6 part by weight of synergistic flower and leaf extract, 4 parts by weight of collagen peptide liposome of preparation example 5, and 100 parts by weight of water.
The preparation method of the synergistic flower and leaf extract comprises the following steps:
taking dried Du Lianhua and perilla leaves, crushing, sieving with a 50-mesh sieve, uniformly mixing according to a mass ratio of 3:1 to obtain a standby raw material, then putting the standby raw material into an ethanol water solution with a mass ratio of 87wt%, stirring and leaching the standby raw material and the ethanol water solution at a speed of 300rpm for 2 hours at 60 ℃, then putting the materials into ultrasonic leaching with ultrasonic frequency of 35kHz and ultrasonic power of 300W for 1 hour, filtering, collecting filtrate, and concentrating under reduced pressure to remove an organic solvent to obtain a crude extract;
A2, adopting H103 type macroporous adsorption resin to adsorb and purify the crude extract, and then washing to remove impurities, wherein the flow rate is 3BV/H; eluting with 45wt% ethanol water solution at flow rate of 2BV/h, collecting eluate, concentrating under reduced pressure to remove organic solvent, and lyophilizing to obtain synergistic extract of flowers and leaves.
The preparation method of the moisturizing and anti-aging cosmetic comprises the following steps:
(1) Uniformly mixing ethylhexyl palmitate, cyclopentasiloxane and C12-15 alcohol benzoate, and heating to 80 ℃ to obtain a phase A; adding carbomer 940, betaine, tridecyl alcohol ether-6, sodium hyaluronate, arginine, allantoin and synergistic flower and leaf extract into water, mixing well, heating to 80deg.C to obtain phase B;
(2) And stirring the phase B at 800rpm for 10min, adding the phase A, continuously stirring for 30min, and continuously stirring for 20min to obtain the moisturizing and anti-aging cosmetic. The lipid oxidation inhibition rate of the moisturizing anti-aging cosmetic of example 7 was 92.90% measured according to the method of test example 1.
The moisturizing and anti-aging cosmetic formula of the embodiment 7 is added with synergistic flower and leaf extracts, preferably Du Lianhua and perilla leaf combinations, and the high-activity moisturizing and anti-aging extracts rich in active ingredients such as phenols, ketones, glycosides and the like are obtained through leaching and purifying processes, so that the moisturizing and anti-aging cosmetic formula has good moisturizing and water locking effects, can effectively promote synthesis of skin collagen, and can assist in enhancing the anti-aging effect of collagen peptide liposome, so that the skin is rich in elasticity and fine wrinkles are prevented.
Test example 1
The anti-aging efficacy evaluation is determined by adopting a lipid oxidation inhibition experiment, and is specifically as follows: taking the moisturizing anti-aging cosmetics prepared in each example as a sample to be tested, firstly, taking 0.5mL of the sample to be tested, placing the sample to be tested in a 10mL test tube with a plug, then sequentially adding 2.5mL of 0.05mol/L phosphate buffer solution with pH=7.0 and 2.5mL of 50mmol/L linoleic acid solution dissolved in 95wt% ethanol, uniformly mixing, then adding 1.25mL of water, uniformly mixing, placing the reaction solution in a biochemical incubator at 45 ℃, and measuring the oxidation degree of the linoleic acid for 48 hours. 0.1mL of the reaction solution was taken, 0.1mL of 30wt% ammonium thiocyanate solution, 4.7mL of 75wt% ethanol solution and 0.1mL of 20mol/L ferrous chloride solution in 3.5wt% hydrochloric acid were sequentially added, and the mixture was shaken and allowed to react for 3 minutes, and the absorbance thereof was measured at a wavelength of 500 nm. The lipid oxidation inhibition rate was calculated as:
lipid oxidation inhibition (%) =100- (a) 48 -A 0 )/(A ’ 48 -A ’ 0 )×100
Wherein A is 0 And A 48 Absorbance of blank of non-added sample at 0h and 48h, A ’ 0 And A ’ 48 To absorbance at 0h and 48h after addition of the test sample.
TABLE 1 anti-aging efficacy test results
| Lipid oxidation inhibition rate% | |
| Example 1 | 77.03 |
| Example 2 | 80.28 |
| Example 3 | 86.42 |
| Example 4 | 86.39 |
| Example 5 | 90.54 |
| Example 6 | 60.76 |
Compared with the collagen peptide used alone in example 6, the elastic nanoliposome used as the carrier of the collagen peptide in example 1 can not only improve the skin permeability of the collagen peptide, but also improve the utilization rate of the collagen peptide and promote the repair of the collagen peptide to the skin. Compared with example 1, the lipid oxidation inhibition ability of example 2 is improved, probably because the crude collagen contains undamaged whole cell tissues, collagen inside the crude collagen cannot be released, and in example 2, the crude collagen is further extracted by adopting ultrasonic, the cell membrane can be effectively destroyed by ultrasonic vibration, the cell content is released, and the cell tissue structure is highly relaxed due to repeated cavitation and impact caused by ultrasonic, and the collagen can be better released after strong homogenization, so that the extraction rate of the collagen can be improved, and the inhibition of the collagen peptide on lipid oxidation is promoted. The lipid oxidation inhibition capability of example 3 is obviously superior to that of example 2, probably because in the preparation process of the nano-liposome, sucrose distearate with two long alkyl chains is used as an edge activator in example 3, so that electrostatic repulsion generated among prepared liposome particles is increased to increase surface charge of the liposome, the resistance which needs to be overcome by aggregation of the liposome is increased, the oxidation speed of the liposome can be slowed down, the stability of the liposome is further increased, meanwhile, the liposome can be filled between bilayer of the liposome, the fluidity of the bilayer is regulated, the melting point of the elastic nano-liposome is effectively reduced, the crystallinity of the nano-liposome is weakened, the membrane fluidity of the nano-liposome is increased, the deformability of the elastic nano-liposome is further increased, the encapsulation efficiency of collagen peptide is improved, meanwhile, the nano-liposome is further facilitated to effectively penetrate through the skin horny layer, and active ingredients are further conveyed into the skin, so that the inhibition capability of the cosmetic on the oxidation of the skin liposome is improved, and the anti-aging effect of the cosmetic is realized.
Test example 2
The whitening efficacy evaluation is determined by tyrosinase inhibition rate experiments, and is specifically as follows: taking the moisturizing anti-aging cosmetics prepared in each example as a sample to be tested, firstly, preparing 100U/mL tyrosinase solution, 0.015 mol/L-tyrosine solution and 0.5mg/mL sample to be tested by using 100mM phosphate buffer solution with pH=6.8; then 1.0mL of the sample solution to be tested, 0.5mL of tyrosinase solution and 2.5mL of 100mM phosphate buffer solution with pH=6.8 are added into a 10mL test tube with a stopper, the mixture is uniformly mixed, the mixture is heated in a water bath at 37 ℃ for 10min, then 1.0mL of L-tyrosine solution is added, the mixture is continuously heated in the water bath at 37 ℃ for 10min, and the absorbance is measured at a wavelength of 475 nm. Each set of examples was tested in parallel for 5 sets and averaged. Tyrosinase activity inhibition rate calculation formula:
tyrosinase inhibition rate= [1- (C-D)/(A-B) ]. Times.100%
Wherein A: absorbance of the solution without the sample solution to be measured and the tyrosinase solution; b: absorbance of the solution without the sample solution to be measured and the tyrosinase solution; c: adding the absorbance of the sample solution to be detected and the tyrosinase solution; d: and adding the absorbance of the sample solution to be tested and the absorbance of the tyrosinase solution not added.
TABLE 2 whitening efficacy test results
| Tyrosinase inhibition rate (%) | |
| Example 1 | 78.10 |
| Example 2 | 82.32 |
| Example 3 | 87.51 |
| Example 4 | 87.48 |
| Example 5 | 91.03 |
| Example 6 | 62.25 |
Tyrosinase is a key enzyme in a series of biochemical reaction steps of melanin biosynthesis, and is prepared by Cu 2+ The metalloenzyme serving as an active center has double functions of oxygenase and oxidase. Collagen peptides in collagen liposomes can effectively sequester Cu 2+ The combination of tyrosine and tyrosinase catalytic active center is hindered, and the oxidation function of tyrosinase is directly inhibited, so that the tyrosinase is inhibited, the melanin content is reduced, and the whitening performance of the cosmetic is realized.
In example 5, both trypsin and subtilisin were used as collagenous hydrolases, which were superior to single trypsin or subtilisin, probably due to the fact that the amino acid residue positions of trypsin hydrolysis are carboxyterminal peptide bonds of glutamic acid, methionine, lysine or glutamine; whereas subtilisin has a strong specificity for the carboxy-terminal hydrophobic amino acids, it recognizes and cleaves the carboxy-terminal peptide bond of aromatic or hydrophobic amino acids such as tyrosine, phenylalanine, tryptophan or leucine. Therefore, the two components are used at the same time, and the two components are synergistic and can be more thoroughly mixed Bottom hydrolysis of collagen improves the yield of collagen peptide, and further has more collagen peptide Cu 2+ Chelation is carried out to prevent the combination of tyrosine and tyrosinase catalytic active center, inhibit the activity of tyrosinase, and further improve the whitening function of the cosmetic.
Claims (9)
1. The preparation method of the collagen peptide liposome is characterized by comprising the following steps:
s1, extracting collagen: washing squid skin with water, taking out, cutting into squid Pi Suikuai, adding into 3-6wt% sodium hydroxide aqueous solution, stirring and leaching for 20-30h, taking out, washing with water to neutrality, and obtaining alkali-treated squid skin; then putting the alkali-treated squid skin into 0.5-2wt% tartaric acid aqueous solution, stirring and leaching for 15-20h, centrifuging, and freeze-drying supernatant to obtain crude collagen; finally adding the crude collagen into ice water, carrying out ultrasonic extraction for 40-80min, centrifuging after the ultrasonic extraction is finished, and freeze-drying supernatant to obtain collagen;
s2, preparation of collagen peptide: adding 8-15 parts by weight of collagen obtained in the step S1 into 25-35 parts by weight of 0.1-0.3mol/L phosphate buffer solution to obtain collagen solution, adding 0.3-0.8 part by weight of hydrolase to perform enzymolysis reaction for 4-6 hours, inactivating the enzyme at 100 ℃ after the enzymolysis reaction is finished, cooling the enzymolysis solution to room temperature, centrifuging, and freeze-drying supernatant to obtain collagen peptide;
S3, preparing collagen peptide liposome: adding 1-3 parts by weight of L-alpha-phosphatidylcholine, 0.2-0.7 part by weight of edge activator and 0.4-1 part by weight of collagen peptide obtained by S2 into 15-25 parts by weight of absolute ethyl alcohol, performing rotary evaporation for 30-50min under the water bath condition of 35-45 ℃, drying for 15-30min in a vacuum drying oven of 35-50 ℃, taking out a lipid membrane, adding 15-25 parts by weight of water, stirring for 10-20min, and performing ultrasonic crushing treatment for 10-20min at 0 ℃ to obtain the collagen peptide liposome.
2. The collagen peptide liposome of claim 1, wherein the hydrolase is one or more of papain, trypsin, aspergillus niger acid protease, pepsin, and subtilisin.
3. The collagen peptide liposome of claim 1, wherein the edge activator is any one of tween 80, sodium cetyl sulfate, cholesterol, sucrose distearate.
4. Collagen peptide liposome prepared by the method of any one of claims 1-3.
5. A moisturizing and anti-aging cosmetic comprising the collagen peptide liposome according to claim 4.
6. The moisturizing and anti-aging cosmetic according to claim 5, comprising the following raw materials in parts by weight: 4-6 parts by weight of ethylhexyl palmitate, 1-3 parts by weight of cyclopentasiloxane, 1.5-2.5 parts by weight of C12-15 alcohol benzoate, 0.4-0.8 part by weight of carbomer 940, 1.5-2.4 parts by weight of betaine, 0.3-0.7 part by weight of emulsifier, 0.2-0.5 part by weight of sodium hyaluronate, 0.1-0.3 part by weight of arginine, 0.2-0.5 part by weight of allantoin, 0.4-0.8 part by weight of synergistic flower and leaf extract, 3-6 parts by weight of collagen peptide liposome and 90-105 parts by weight of water.
7. The moisturizing and anti-aging cosmetic according to claim 6, wherein the synergistic flower and leaf extract is prepared by the following steps:
taking dried Du Lianhua and perilla leaves, crushing and sieving, uniformly mixing according to the mass ratio of 3 (1-2) to obtain a standby raw material, then putting the standby raw material into an ethanol water solution with the mass ratio of 82-88wt%, wherein the mass ratio of the standby raw material to the ethanol water solution is 1 (7-10), stirring and leaching at the temperature of 55-65 ℃ at the rotating speed of 200-300rpm for 2-3h, then putting the materials into ultrasonic wave with the ultrasonic frequency of 30-40kHz and the ultrasonic power of 300-500W for ultrasonic leaching for 1-2h, filtering, collecting filtrate, decompressing and concentrating to remove an organic solvent, thus obtaining a crude extract;
a2, adopting macroporous adsorption resin to adsorb and purify the crude extract, and then washing to remove impurities, wherein the flow rate is 2-3BV/h; eluting with 40-50wt% ethanol water solution at flow rate of 2-3BV/h, collecting eluate, concentrating under reduced pressure to remove organic solvent, and freeze drying to obtain synergistic flower and leaf extract.
8. The moisturizing and anti-aging cosmetic according to claim 6, wherein the emulsifier is any one of tridecyl alcohol ether-6, glyceryl monostearate, polyoxyethylene stearate, sorbitan stearate 165.
9. The method for preparing a moisturizing and anti-aging cosmetic according to any one of claims 6 to 8, comprising the steps of:
(1) Uniformly mixing ethylhexyl palmitate, cyclopentasiloxane and C12-15 alcohol benzoate to obtain a phase A; adding carbomer 940, betaine, emulsifier, sodium hyaluronate, arginine, allantoin, and synergistic folium Phyllostachydis Henonis extract into water, and mixing to obtain phase B;
(2) And stirring the phase B for 8-12min, and adding the phase A and the liposome to obtain the moisturizing and anti-aging cosmetic.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117426996A (en) * | 2023-11-24 | 2024-01-23 | 星购(天津)科技有限公司 | Anti-wrinkle peptide composition and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117426996A (en) * | 2023-11-24 | 2024-01-23 | 星购(天津)科技有限公司 | Anti-wrinkle peptide composition and preparation method thereof |
| CN117426996B (en) * | 2023-11-24 | 2024-04-02 | 星购(天津)科技有限公司 | Anti-wrinkle peptide composition and preparation method thereof |
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Application publication date: 20231110 |