CN112263505A - Copper peptide composition and preparation method and application thereof - Google Patents
Copper peptide composition and preparation method and application thereof Download PDFInfo
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- CN112263505A CN112263505A CN202011183721.2A CN202011183721A CN112263505A CN 112263505 A CN112263505 A CN 112263505A CN 202011183721 A CN202011183721 A CN 202011183721A CN 112263505 A CN112263505 A CN 112263505A
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- copper
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- MVORZMQFXBLMHM-QWRGUYRKSA-N Gly-His-Lys Chemical compound NCCCC[C@@H](C(O)=O)NC(=O)[C@@H](NC(=O)CN)CC1=CN=CN1 MVORZMQFXBLMHM-QWRGUYRKSA-N 0.000 title claims abstract description 127
- 238000002360 preparation method Methods 0.000 title claims abstract description 91
- 239000000203 mixture Substances 0.000 title claims abstract description 71
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
- 150000001879 copper Chemical class 0.000 claims abstract description 17
- 238000004108 freeze drying Methods 0.000 claims description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 15
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 15
- 229930195725 Mannitol Natural products 0.000 claims description 15
- 239000010949 copper Substances 0.000 claims description 15
- 229910052802 copper Inorganic materials 0.000 claims description 15
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- 235000010355 mannitol Nutrition 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- OCUCCJIRFHNWBP-IYEMJOQQSA-L Copper gluconate Chemical compound [Cu+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O OCUCCJIRFHNWBP-IYEMJOQQSA-L 0.000 claims description 13
- 229940108925 copper gluconate Drugs 0.000 claims description 13
- 239000002537 cosmetic Substances 0.000 claims description 13
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- HDTRYLNUVZCQOY-UHFFFAOYSA-N α-D-glucopyranosyl-α-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OC1C(O)C(O)C(O)C(CO)O1 HDTRYLNUVZCQOY-UHFFFAOYSA-N 0.000 claims description 7
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- PNNNRSAQSRJVSB-UHFFFAOYSA-N L-rhamnose Natural products CC(O)C(O)C(O)C(O)C=O PNNNRSAQSRJVSB-UHFFFAOYSA-N 0.000 claims description 7
- HDTRYLNUVZCQOY-WSWWMNSNSA-N Trehalose Natural products O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-WSWWMNSNSA-N 0.000 claims description 7
- HDTRYLNUVZCQOY-LIZSDCNHSA-N alpha,alpha-trehalose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-LIZSDCNHSA-N 0.000 claims description 6
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- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 5
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 5
- LHBCBDOIAVIYJI-DKWTVANSSA-L copper;(2s)-2-aminobutanedioate Chemical compound [Cu+2].[O-]C(=O)[C@@H](N)CC([O-])=O LHBCBDOIAVIYJI-DKWTVANSSA-L 0.000 claims description 5
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 4
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- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 9
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Images
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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/64—Proteins; Peptides; Derivatives or degradation products 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
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/20—Halogens; Compounds 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
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/23—Sulfur; Selenium; Tellurium; Compounds 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
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/36—Carboxylic acids; Salts or anhydrides thereof
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- A—HUMAN NECESSITIES
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- 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
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/36—Carboxylic acids; Salts or anhydrides thereof
- A61K8/365—Hydroxycarboxylic acids; Ketocarboxylic acids
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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
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives 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
- A61Q19/08—Anti-ageing preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/88—Two- or multipart kits
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Public Health (AREA)
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- Inorganic Chemistry (AREA)
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- Gerontology & Geriatric Medicine (AREA)
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- Medicines That Contain Protein Lipid Enzymes And Other Medicines (AREA)
Abstract
The invention provides a copper peptide composition and a preparation method and application thereof, wherein the copper peptide composition comprises an A component and a B component which are independently packaged; the A component comprises tripeptide-1; the component B comprises copper salt and water. The copper peptide composition provided by the invention is safe and harmless, has an obvious anti-aging effect, and can be stably stored for a long time.
Description
Technical Field
The invention belongs to the field of daily chemicals, particularly relates to a copper peptide composition and a preparation method and application thereof, and particularly relates to a high-activity high-stability copper peptide composition and a preparation method and application thereof.
Background
The blue copper peptide (tripeptide-1 copper, copper peptide, GHK-Cu) is a complex compound formed by complexing small molecular peptides and divalent copper ions, is composed of glycine-histidine-lysine-copper, has the functions of promoting wound healing, resisting oxidation, promoting regeneration of collagen and elastin, resisting inflammation and the like, and is widely applied to the cosmetic industry.
The tripeptide-1 (GHK) and the divalent copper ion have a strong affinity. GHK-Cu exerts its active function in the form of a complex. GHK-Cu can accelerate wound healing and contraction, and improve the acceptance of the body to the transplanted skin; stimulating the production of glycosaminoglycans (GAGs), helping the skin to restore its ability to repair itself; activates the synthesis of collagen dermatan sulfate chitin and small molecule glycoprotein. In addition, GHK-Cu can increase the thickness of epidermis and dermis, increase skin elasticity, reduce wrinkles, and remove skin blemishes such as color spots and sunburn marks.
The effect of GHK-Cu is achieved by its complex form. It is believed that GHK transports copper ions into cells in a non-toxic form and enables their use by cells by forming GHK-Cu complexes. Copper is an essential trace element for human body, and many important enzymes in human body need copper ions to influence the formation of tissues, oxidation resistance and cell behavior and metabolism; however, excessive free copper ions in the blood can cause damage to the liver. Therefore, from the viewpoint of efficacy and safety, it is important to protect the integrity of the GHK-Cu complex in practical use.
In the field of cosmetics, GHK-Cu is directly applied to products such as essence, freeze-dried powder, cream and the like as a ready-made raw material. However, the GHK-Cu complex is easy to hydrolyze under the oxidation condition; in addition, the acidic substances can easily free copper ions in the GHK-Cu, so that the skin care effect of the blue copper peptide is greatly reduced. The copper peptide product is influenced by the environment and temperature change in the transportation and storage processes, so that the GHK-Cu compound in the product is decomposed possibly, and the efficacy of the product is influenced.
CN110840786A discloses a blue copper peptide essence and a preparation method thereof, wherein the blue copper peptide essence comprises the following raw materials: water, glycerin, hydrolyzed collagen, euglena gracilis polysaccharide, maltooligosaccharide glucoside, hydrogenated starch hydrolysate, tripeptide-1 copper, acetyl hexapeptide-8, dipeptide-1, dipeptide-2, sodium hyaluronate, trehalose, prickly pear stem extract, prickly ash fruit extract, 1, 2-pentanediol, pomelo fruit extract, hamamelis virginiana extract, arginine and imidazolidinyl urea. The tripeptide-1 copper and other active substances are directly added to achieve the effects of resisting wrinkles, delaying aging and repairing skin, but the tripeptide-1 copper in a liquid phase system is easy to hydrolyze, so that the tripeptide-1 is separated from copper ions, and the activity and the efficacy of the composition are possibly reduced.
CN109512691A discloses a blue copper peptide freeze-dried powder preparation and a preparation method thereof, comprising a solution agent composed of blue copper peptide freeze-dried powder and blue copper peptide lysozyme solution, wherein the blue copper peptide freeze-dried powder is prepared from the following components in parts by weight: tripeptide-1 copper, mannitol, sodium hyaluronate, oligopeptide-1 and water; the bluecopper peptide freeze-dried powder lysozyme is prepared from the following components in parts by weight: glycerol, 1, 3-butanediol small nucleus (scleritium rolfsii) gelatin, pentapeptide-1, PGA-WS polyglutamic acid, sodium hyaluronate, GC-04 extract, essence, placenta (animal) protein, and water. However, the tripeptide-1 copper in the freeze-dried powder preparation has the possibility of being decomposed in the storage process, and the activity of the preparation is influenced.
CN110237007A discloses a cosmetic composition containing blue copper peptide, a preparation method and application thereof. The cosmetic composition comprises the following components in parts by weight: blueish peptides, purslane extract, VB5, centella asiatica extract. The composition obtained by mixing the bluepatilin, the purslane extract, the VB5 and the centella extract can play the relieving and anti-allergy effects of all the components, and when the composition is applied to cosmetics, the dosage of a chemical synthetic preparation with the relieving and anti-allergy effects can be obviously reduced, so that the relieving and anti-allergy effects are good, the irritation is small, and the effects of diminishing inflammation, moisturizing and repairing are also achieved. However, there is also a problem that degradation of copper peptide leads to a decrease in activity.
GHK-Cu is directly applied to products such as essence, freeze-dried powder and face cream as a ready-made raw material, and has the functions of promoting wound healing, resisting oxidation, promoting regeneration of collagen and elastin, resisting inflammation and the like. However, the peptide product is affected by the environmental and temperature changes during transportation and storage, and the GHK-Cu complex in the product may be decomposed, which affects the efficacy of the product. Therefore, how to provide a safe, efficient and stable copper peptide composition becomes a problem to be solved urgently.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a copper peptide composition and a preparation method and application thereof, and particularly provides a copper peptide composition with high activity and high stability and a preparation method and application thereof. The copper peptide composition provided by the invention is safe and harmless, has an obvious anti-aging effect, and can be stably stored for a long time.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a copper peptide composition comprising separately packaged a and B components.
The A component comprises tripeptide-1.
The component B comprises copper salt and water.
The copper peptide composition composed of the specific components is safe and harmless, and has a remarkable anti-aging effect. The tripeptide-1 component and the copper salt component are separated by adopting an independent packaging mode, and the A component and the B component are mixed to complex the tripeptide-1 and the copper salt to form the copper peptide when in use, so that the freshness and the activity of the copper peptide are ensured, the problem of activity reduction caused by decomposition of the copper peptide due to long-term storage is avoided, the use feeling of a consumer on the composition is enhanced, and the interestingness in the use process is enriched.
Preferably, the a component further comprises water.
Preferably, the component A comprises tripeptide-10.1-7 parts by weight and water 85-99.9 parts by weight.
The amount of tripeptide-1 may be 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, 1 part, 1.5 parts, 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts, 6.5 parts, or 7 parts, and the amount of water may be 85 parts, 86 parts, 87 parts, 88 parts, 89 parts, 90 parts, 91 parts, 92 parts, 93 parts, 94 parts, 95 parts, 96 parts, 97 parts, 98 parts, 99 parts, 99.5 parts, or 99.9 parts, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned ranges are also applicable.
Preferably, the a component further comprises an excipient.
The excipient can fully disperse the solid tripeptide-1, and is convenient to use.
Preferably, the excipient comprises any one or a combination of at least two of mannitol, rhamnose or trehalose, such as a combination of mannitol and rhamnose, a combination of rhamnose and trehalose or a combination of trehalose and mannitol, etc., but is not limited to the listed combinations, and other combinations not listed within the above-mentioned combination range are also applicable.
Preferably, the component A comprises tripeptide-10.1-7 parts and excipient 3-7 parts in parts by weight. The tripeptide-1 may be used in an amount of 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, 1 part, 1.5 part, 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts, 6.5 parts or 7 parts, and the excipient may be used in an amount of 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts, 6.5 parts or 7 parts, but the amount is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned ranges are also applicable.
The combination of the above specific numerical ranges enables better dispersion of the tripeptide-1 for convenient use by people.
Preferably, the component B comprises 0.1-7 parts by weight of copper salt and 70-99.5 parts by weight of water. The amount of the copper salt may be 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, 1 part, 1.5 part, 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts, 6.5 parts, or 7 parts, and the amount of water may be 70 parts, 72 parts, 74 parts, 76 parts, 78 parts, 80 parts, 82 parts, 84 parts, 86 parts, 88 parts, 90 parts, 92 parts, 94 parts, 96 parts, 98 parts, 99 parts, 99.1 parts, 99.2 parts, 99.3 parts, 99.4 parts, or 99.5 parts, but is not limited to the recited values, and other values not recited in the above numerical ranges are also applicable.
Preferably, the copper salt includes any one or a combination of at least two of copper gluconate, copper aspartate, copper sulfate, copper chloride, copper acetate, or copper acetomethionate, such as a combination of copper gluconate and copper aspartate, a combination of copper aspartate and copper sulfate, a combination of copper sulfate and copper chloride, or a combination of copper chloride and copper acetate, and the like, but is not limited to the listed combinations, and other combinations not listed in the above-mentioned combination range are also applicable.
The specific copper salt can rapidly form a copper peptide complex with tripeptide-1, and is convenient for people to use.
In a second aspect, the present invention provides a method for preparing a copper peptide composition as described above, comprising the steps of: dissolving tripeptide-1 and excipients in water, followed by lyophilization to obtain the a component; and dissolving copper salt in water to obtain the component B.
The copper peptide composition prepared by the method has high activity, safety, harmlessness and remarkable anti-aging effect, and can be stably stored for a long time.
Preferably, the freeze-drying process comprises the steps of reducing the pressure to 10-30 Pa, carrying out first freeze-drying for 2-3 h at-45 to-40 ℃, then carrying out second freeze-drying for 10-15 h at-17 to-12 ℃ for the first time, then carrying out second freeze-drying for 30-35 ℃ for the second time, and standing for 3-5 h.
Wherein, the pressure can be 10Pa, 12Pa, 14Pa, 16Pa, 18Pa, 20Pa, 22Pa, 24Pa, 26Pa, 28Pa or 30Pa, the first freeze-drying temperature can be-45 ℃, -44 ℃, -43 ℃, -42 ℃, -41 ℃ or-40 ℃, the first freeze-drying time can be 2h, 2.2h, 2.4h, 2.6h, 2.8h or 3h, the first temperature can be-17 ℃, -16 ℃, -15 ℃, -14 ℃, -13 ℃ or-12 ℃ and the like, the second freeze-drying time can be 10h, 11h, 12h, 13h, 14h or 15h and the like, the second temperature can be 30 ℃, 31 ℃, 32 ℃, 33 ℃, 34 ℃ or 35 ℃ and the like, the standing time can be 3h, 3.5h, 4h, 4.5h or 5h and the like, but is not limited to the recited values, other values not listed in the above numerical ranges are also applicable.
As a preferred technical scheme of the invention, the preparation method comprises the following steps: dissolving tripeptide-1 and an excipient in water, then decompressing to 10-30 Pa, carrying out primary freeze-drying for 2-3 h at-45 to-40 ℃, then heating to-17 to-12 ℃ for the first time, carrying out secondary freeze-drying for 10-15 h, then heating to 30-35 ℃ for the second time, and standing for 3-5 h to obtain a component A; and dissolving copper salt in water to obtain the component B.
In a third aspect, the invention also provides the application of the copper peptide composition in preparing cosmetics.
Preferably, the cosmetic comprises a lotion, essence, cream, skin lotion or eye cream.
Compared with the prior art, the invention has the following beneficial effects:
the copper peptide composition provided by the invention is safe and harmless, has an obvious anti-aging effect, and the wrinkle change rate reaches-1.63% from continuous use to eighth week; the tripeptide-1 component and the copper salt component are separated by adopting an independent packaging mode, and the A component and the B component are mixed to complex the tripeptide-1 and the copper salt to form the copper peptide when in use, so that the freshness and the activity of the copper peptide are ensured, the problem of activity reduction caused by decomposition of the copper peptide due to long-term storage is avoided, the use feeling of a consumer on the composition is enhanced, and the interestingness in the use process is enriched.
Drawings
FIG. 1 is a liquid chromatogram of the copper peptide composition provided in preparation example 1;
fig. 2 is a liquid chromatogram of the copper peptide solution provided in comparative example 1.
Detailed Description
To further illustrate the technical means and effects of the present invention, the following further describes the technical solution of the present invention with reference to the preferred application examples of the present invention, but the present invention is not limited to the scope of the application examples.
Preparation example 1
The preparation example provides a copper peptide composition, which comprises the following components in parts by weight:
the component A comprises: tripeptide-13.5 parts and water 88 parts;
and B component: 3.5 parts of copper gluconate and 75.5 parts of water.
The preparation method comprises the following steps: dissolving tripeptide-1 in water to obtain a component A; the copper gluconate was dissolved in water to obtain the B component.
Preparation example 2
The preparation example provides a copper peptide composition, which comprises the following components in parts by weight:
the component A comprises: tripeptide-10.5 parts, water 91 parts;
and B component: 0.5 part of copper chloride and 78.5 parts of water.
The preparation method is the same as that of preparation example 1.
Preparation example 3
The preparation example provides a copper peptide composition, which comprises the following components in parts by weight:
the component A comprises: tripeptide-15 parts and water 86.5 parts;
and B component: 5 parts of copper aspartate and 74 parts of water.
The preparation method is the same as that of preparation example 1.
Preparation example 4
The preparation example provides a copper peptide composition, which comprises the following components in parts by weight:
the component A comprises: tripeptide-10.1 parts, water 91.4 parts;
and B component: copper sulfate 0.1 weight portions and water 78.9 weight portions.
The preparation method is the same as that of preparation example 1.
Preparation example 5
The preparation example provides a copper peptide composition, which comprises the following components in parts by weight:
the component A comprises: tripeptide-17 parts and water 84.5 parts;
and B component: copper acetate 7 parts and water 72 parts.
The preparation method is the same as that of preparation example 1.
Preparation example 6
The preparation example provides a copper peptide composition, which comprises the following components in parts by weight:
the component A comprises: tripeptide-13.5 parts, mannitol 5 parts;
and B component: 3.5 parts of copper gluconate and 75.5 parts of water.
The preparation method comprises the following steps: dissolving tripeptide-1 and mannitol in water, and then freeze-drying at-45 ℃ for 2 hours at the pressure of 20Pa for the first time; the second freeze-drying temperature is-15 ℃ and the time is 10 hours; standing at 35 deg.C for 4h to freeze-dry the composition to obtain component A; copper gluconate was dissolved in water to obtain component B.
Preparation example 7
The preparation example provides a copper peptide composition, which comprises the following components in parts by weight:
the component A comprises: tripeptide-10.5 parts, rhamnose 4 parts;
and B component: 0.5 part of copper gluconate and 78.5 parts of water.
The preparation method comprises the following steps: dissolving tripeptide-1 and mannitol in water, and then freeze-drying at-43 ℃ for 2.5h under the pressure of 10Pa for the first time; the second freeze-drying temperature is-17 ℃ and the time is 13 h; standing at 32 deg.C for 3h to freeze-dry the composition to obtain component A; copper gluconate was dissolved in water to obtain component B.
Preparation example 8
The preparation example provides a copper peptide composition, which comprises the following components in parts by weight:
the component A comprises: tripeptide-15 parts and trehalose 6 parts;
and B component: 5 parts of copper gluconate and 74 parts of water.
The preparation method comprises the following steps: dissolving tripeptide-1 and mannitol in water, and then freeze-drying at-40 ℃ for 3h under the pressure of 30Pa for the first time; the second freeze-drying temperature is-10 ℃ and the time is 15 h; standing at 30 deg.C for 5h to freeze-dry the composition to obtain component A; copper gluconate was dissolved in water to obtain component B.
Preparation example 9
The preparation example provides a copper peptide composition, which comprises the following components in parts by weight:
the component A comprises: tripeptide-10.1 parts, mannitol 1 part and rhamnose 2 parts;
and B component: 0.1 part of copper gluconate and 78.9 parts of water.
The preparation method is the same as that of preparation example 6.
Preparation example 10
The preparation example provides a copper peptide composition, which comprises the following components in parts by weight:
the component A comprises: tripeptide-17 parts, mannitol 7 parts;
and B component: 7 parts of copper gluconate and 72 parts of water.
The preparation method is the same as that of preparation example 6.
Preparation example 11
This preparation example provides a copper peptide composition, which is the same as that of preparation example 6 except that mannitol was replaced with an equal amount of rhamnose as compared with preparation example 6.
The preparation method is the same as that of preparation example 6.
Preparation example 12
This preparation example provides a copper peptide composition, which is the same as that of preparation example 6 except that mannitol was replaced with trehalose in an amount equivalent to that of preparation example 6.
The preparation method is the same as that of preparation example 6.
Comparative example 1
The comparative example provides a copper peptide solution, which comprises the following components in parts by weight:
tripeptide-1 copper 3.5 parts, water 163.5 parts.
Application example 1
The application example provides essence containing the copper peptide composition provided in preparation example 1, and the essence comprises the following components in parts by weight:
the preparation method comprises the following steps: mixing and stirring the component A of the copper peptide composition provided by the preparation example 1, glycerol, butanediol, sodium hyaluronate and p-hydroxyacetophenone uniformly to obtain a phase A; the B component of the cupeptide composition provided in preparation example 1, glycerol glucoside and glycerol were mixed and stirred uniformly to obtain phase B.
Application examples 2 to 5
Application examples 2 to 5 were compared with application example 1, except that the A-component of the copper peptide composition provided in preparation example 1 in the A-phase was replaced with the A-component of the copper peptide composition provided in preparation examples 2 to 5 in the same amount, respectively, and the B-component of the copper peptide composition provided in preparation example 1 in the B-phase was replaced with the B-component of the copper peptide composition provided in preparation examples 2 to 5 in the same amount, respectively.
The preparation method is the same as application example 1.
Application example 6
The application example provides freeze-dried powder containing the copper peptide composition provided in preparation example 6, and the freeze-dried powder comprises the following components in parts by weight:
phase A: preparation example 6 provides component a of the copper peptide composition;
phase B: preparation example 6 provides 79 parts of component B, 1 part of glycerol glucoside and 20 parts of glycerol.
The preparation method comprises the following steps: phase a is component a of the copper peptide composition provided in preparative example 6; the B component of the cupeptide composition provided in preparation example 6, glycerol glucoside and glycerol were mixed and stirred uniformly to obtain phase B.
Application examples 7 to 10
Application examples 7 to 10 were compared with application example 6, and the same as in application example 6 except that the A-component of the copper peptide composition provided in production example 6 in the A-phase was replaced with the A-component of the copper peptide composition provided in production examples 7 to 10, respectively, and the B-component of the copper peptide composition provided in production example 6 in the B-phase was replaced with the B-component of the copper peptide composition provided in production examples 7 to 10, respectively, in equal amounts.
The preparation method is the same as in application example 6.
Application examples 11 to 12
Application examples 11 to 12 were compared with application example 6, and the same as application example 6 except that the A-component of the copper peptide composition provided in preparation example 6 in the B phase was replaced with the A-component of the copper peptide composition provided in preparation examples 11 to 12 in the same amounts, respectively.
The preparation method is the same as in application example 6.
Comparative application example 1
The comparative application example provides an essence containing the blue copper peptide, wherein the copper peptide solution provided in the comparative example 1 is directly added, and the components and the parts by weight of the copper peptide solution are as follows:
the preparation method comprises the following steps: and mixing tripeptide-1 copper, glycerol, butanediol, sodium hyaluronate, p-hydroxyacetophenone, glycerol glucoside and water, and stirring uniformly to obtain the essence containing the bluecopper peptide.
Comparative application example 2
The comparative application example provides a freeze-dried powder containing the blue copper peptide, wherein tripeptide-1 copper is directly added, and the components and the parts by weight of the tripeptide-1 copper are as follows:
phase A: 7 parts of tripeptide-1 copper and 5 parts of mannitol;
phase B: 75.5 parts of water, 1 part of glycerol glucoside and 20 parts of glycerol.
The preparation method comprises the following steps: dissolving tripeptide-1 copper and mannitol in water, and then carrying out first freeze-drying at the temperature of-45 ℃ for 2h under the pressure of 20 Pa; the second freeze-drying temperature is-15 ℃ and the time is 10 hours; standing at 35 deg.C for 4h to freeze-dry the composition to obtain phase A; mixing water, glycerol glucoside and glycerol, and stirring to obtain phase B.
Pretreatment before testing
Before the copper peptide content test, the safety test and the anti-aging test, the cosmetics of application examples 1 to 12 and comparative application examples 1 to 2 which are required to be used in the test are subjected to test pretreatment.
The instrument comprises the following steps: a constant-temperature incubator: the temperature control precision is +/-1 ℃.
The treatment method comprises the following steps: the experimental method comprises the following steps: putting the sample into a constant temperature incubator with the preset adjusted temperature of 48 +/-1 ℃, taking out the sample after 48 hours, and carrying out other tests on the product after the temperature is recovered to the room temperature.
Copper peptide content test
The purpose of the test is as follows: the products provided by preparation example 1 and comparative example 1 which are subjected to experimental pretreatment are subjected to liquid chromatography analysis, and the relative content difference is detected.
The test instrument: shimadzu LC20A, column C18.
The test conditions are as follows: the mobile phase (methanol + water (5% + 95%), 5% methanol was raised to 10% over 10 minutes, maintained for 3 minutes, then lowered from 10% methanol to 5% over 7 minutes, flow rate (0.8mL/min), column temperature 30 ℃, sample size 10. mu.L.
And (3) test results: FIG. 1 shows the chromatogram results of preparation example 1; comparative example 1 the chromatogram results are shown in figure 2. The copper peptide content of the sample is indicated by the peak area, and the peak area data are shown in table 1.
TABLE 1
| Sample (I) | |
Total peak surface | Ratio of occupation of |
| Preparation example 1 | 496209 | 502751 | 98.70％ |
| Comparative example 1 | 459911 | 491383 | 93.60％ |
The above results show that the content of copper peptide in preparation example 1 is higher than that in comparative example 1. The result shows that the tripeptide-1 and the copper ions are separately and independently packaged, and the tripeptide-1 and the copper ions are compounded to prepare the copper peptide when in use, so that the copper peptide has better stability.
Safety test
The purpose of the test is as follows: safety tests were performed on the products provided in application examples 1-12 and comparative application examples 1-2.
Subject: 150 subjects were selected and randomized into 150 groups of 10 individuals each aged 18-24 years without allergic history.
The specific method comprises the following steps: the closed patch test is carried out for 48 h. The cosmetics 20mg provided in application examples 1 to 12 and comparative application examples 1 to 2 were weighed into a spot tester, respectively, while setting a blank control (nothing added). Cleaning the inner side of the arm of the subject, sticking the plaque test device with the sample on the selected position of the inner side of the arm of the subject by using a non-irritating adhesive tape, and lightly pressing the plaque test device with fingers after sticking the plaque test device on the skin for 48 hours. The stung subject keeps the spot patch part dry within 48h, and avoids violent exercise, scratching spot test part, long-time sunlight irradiation and the like. And after 48h, removing the tester and marking, after 30min, judging under sufficient light after the pressure marks disappear, and respectively carrying out revisit observation within 72h and 96 h. The skin adverse reaction grading criteria are shown in table 2:
TABLE 2
The test results are shown in table 3:
TABLE 3
The results show that the product provided by the invention is safe and harmless.
Facial fine line test
The purpose of the test is as follows: the anti-aging efficacy test was performed on the cosmetics provided in application examples 1 to 12 and comparative application examples 1 to 2.
An experimental instrument: digital skin image analyzer Derma Vision-PRO.
Subject: 308 subjects, age 30-40, were selected and randomized into 14 groups (22 individuals per group) using the cosmetics provided in application examples 1-12 and comparative application examples 1-2, respectively.
The test method comprises the following steps: (1) after washing the face of a subject, resting for 30 minutes in a constant temperature and humidity chamber (the ambient temperature is 21 +/-1 ℃ and the relative humidity is 45 +/-5%), and shooting fine line pictures of the front face and the side face of the subject by using a digital skin image analyzer; (2) issuing a test sample, informing a product using method, bringing the test sample back to use by a subject, using the test sample once in the morning and at night, and regularly checking a card to record the use; (3) the product is used for 8 weeks, and the fine lines on the face are photographed every two weeks for 5 times in total, namely, the fine lines are measured once every 0 week, 2 weeks, 4 weeks, 6 weeks and 8 weeks.
The results of the tests are obtained from instrumental analyses and are shown in tables 4 and 5, where the data are presented as averages:
table 4 wrinkle proportion at each stage (%)
TABLE 5 wrinkle Change Rate (%) at each stage
As can be seen from the data in the table, compared with the comparative application example, the product provided by the invention has low wrinkle ratio and high wrinkle ratio reduction rate, and fully shows that the A, B component independently packaged copper peptide composition provided by the invention has the characteristics of high anti-aging capacity and high stability.
The applicant states that the copper peptide composition, the preparation method and the application thereof are described by the application examples, but the invention is not limited to the application examples, namely, the invention is not meant to be dependent on the application examples to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
Claims (10)
1. A copper peptide composition, wherein the copper peptide composition comprises a component a and a component B packaged separately;
the A component comprises tripeptide-1;
the component B comprises copper salt and water.
2. The copper peptide composition of claim 1, wherein the a component further comprises water.
3. The copper peptide composition of claim 2, wherein the component A comprises tripeptide-10.1-7 parts by weight and water 85-99.9 parts by weight.
4. The copper peptide composition of claim 1, wherein the a component further comprises an excipient;
preferably, the excipient comprises any one or a combination of at least two of mannitol, rhamnose or trehalose;
preferably, the component A comprises tripeptide-10.1-7 parts and excipient 3-7 parts in parts by weight.
5. The copper peptide composition as claimed in any one of claims 1 to 4, wherein the component B comprises 0.1 to 7 parts by weight of copper salt and 70 to 99.5 parts by weight of water.
6. The copper peptide composition of any one of claims 1-5, wherein the copper salt comprises any one of copper gluconate, copper aspartate, copper sulfate, copper chloride, copper acetate, or copper acetomethionate, or a combination of at least two thereof.
7. The method of claim 4, wherein the method of preparing the copper peptide composition comprises the steps of: dissolving tripeptide-1 and excipients in water, followed by lyophilization to obtain the a component; and dissolving copper salt in water to obtain the component B.
8. The preparation method of the copper peptide composition according to claim 7, wherein the freeze-drying process comprises the steps of reducing pressure to 10-30 Pa, carrying out first freeze-drying at-45-40 ℃ for 2-3 h, then carrying out second freeze-drying at-17-12 ℃ for 10-15 h, then carrying out second temperature rise to 30-35 ℃, and standing for 3-5 h.
9. The method of preparing a copper peptide composition according to claim 7 or 8, wherein said method comprises the steps of: dissolving tripeptide-1 and an excipient in water, then decompressing to 10-30 Pa, carrying out primary freeze-drying for 2-3 h at-45 to-40 ℃, then heating to-17 to-12 ℃ for the first time, carrying out secondary freeze-drying for 10-15 h, then heating to 30-35 ℃ for the second time, and standing for 3-5 h to obtain a component A; and dissolving copper salt in water to obtain the component B.
10. Use of a copper peptide composition according to any one of claims 1 to 6 for the preparation of a cosmetic;
preferably, the cosmetic comprises a lotion, essence, cream, skin lotion or eye cream.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114907442A (en) * | 2022-06-08 | 2022-08-16 | 常熟理工学院 | Organic silicon modified copper peptide and preparation method thereof |
| CN115025001A (en) * | 2022-05-31 | 2022-09-09 | 陕西慧康生物科技有限责任公司 | Peptide composition with multiple whitening and freckle removing effects and application thereof |
| CN117126230A (en) * | 2023-10-23 | 2023-11-28 | 广州同隽医药科技有限公司 | Synthesis method and application of tripeptide-1 and blue copper peptide |
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| CN117126230A (en) * | 2023-10-23 | 2023-11-28 | 广州同隽医药科技有限公司 | Synthesis method and application of tripeptide-1 and blue copper peptide |
| CN117126230B (en) * | 2023-10-23 | 2024-02-13 | 广州同隽医药科技有限公司 | Synthesis method and application of tripeptide-1 and blue copper peptide |
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Application publication date: 20210126 |