CN113549665A - Oligopeptide compound, preparation method thereof and prepared anti-wrinkle repair emulsion - Google Patents

Oligopeptide compound, preparation method thereof and prepared anti-wrinkle repair emulsion Download PDF

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CN113549665A
CN113549665A CN202110844580.2A CN202110844580A CN113549665A CN 113549665 A CN113549665 A CN 113549665A CN 202110844580 A CN202110844580 A CN 202110844580A CN 113549665 A CN113549665 A CN 113549665A
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廖望
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Abstract

The invention provides an oligopeptide compound, a preparation method thereof and a prepared anti-wrinkle repair emulsion, belonging to the technical field of cosmetics, wherein the anti-wrinkle emulsion comprises the following components in percentage by mass: 1-3% of sorbitan laurate, 2-4% of glycerol, 1-2.5% of 1, 2-propylene glycol, 0.01-0.04% of EDTA disodium, 2-4% of glyceryl caprylate, 0.1-0.7% of sodium dihydrogen phosphate, 2-5% of oligopeptide compound, 101-3% of coenzyme Q, and the balance of purified water. The preparation method is simple, can improve pimples and solar injuries, can obviously repair damaged cells, smooth fine lines and has obvious effects of resisting wrinkles and ageing.

Description

Oligopeptide compound, preparation method thereof and prepared anti-wrinkle repair emulsion
Technical Field
The invention relates to the technical field of cosmetics, in particular to an oligopeptide compound, a preparation method thereof and a prepared anti-wrinkle repair emulsion.
Background
Aging is one of the most undesirable problems that everyone wants to have a young face. Therefore, anti-aging is a constant pursuit of beauty consumers. Wrinkles usually appear only due to aging, but now, the wrinkles are more and more aged, and the lower head is rather popular with wrinkle men. It can be seen that the generation of wrinkles has no absolute relation with age, and is more originated from people's habits. Perhaps when the face of the person is young and tight, the wrinkles appear quietly. The more wrinkles, the older. More and more people are concerned about wrinkles in T-shaped areas, and how to fade the wrinkles and relieve the wrinkles becomes more and more important.
At present, a lot of products for promoting wrinkle removal and wrinkle resistance exist, but a lot of comfortable and good-effect optional products do not exist. Many products with anti-wrinkle and wrinkle-removing effects have only simple relieving effects, and cannot realize effective deep repair of skin, so that wrinkles cannot be faded and removed fundamentally. In addition, many existing care products have anti-wrinkle and wrinkle-removing effects, which are usually added to other care products, such as facial masks or isolation creams, etc., as auxiliary functions, wherein the main functions are moisturizing and sun-screening, while the anti-wrinkle and wrinkle-removing effects are more and more added as additional added effects, and the actually generated anti-wrinkle and wrinkle-removing effects are very slight. In addition, in many existing products with anti-wrinkle and anti-wrinkle effects, such as facial masks or isolation creams, essence and/or pigment are often added, and compounds and heavy metals contained in the products can remain on the skin to cause pollution and damage to the skin, but rather make the skin of people more prone to aging, which is not beneficial to improving the skin.
Disclosure of Invention
The invention aims to provide an oligopeptide compound, a preparation method thereof and a prepared anti-wrinkle repair emulsion, overcomes the defects and shortcomings of existing wrinkle removal and anti-aging, and provides an anti-wrinkle repair product capable of effectively improving the depth of deep wrinkles, reducing the number of wrinkles and improving skin nutrition.
The technical scheme of the invention is realized as follows:
the invention provides a preparation method of an oligopeptide compound, which comprises the following steps:
s1, cleaning the whole chlamys farreri meat, adding distilled water, and homogenizing to obtain slurry; then, cleaning and crushing deep sea fish scales to obtain fish scale powder; uniformly mixing the fish scale powder and the slurry for later use;
s2, adding papain and chymotrypsin in the step S1, performing enzymolysis, and inactivating enzyme to obtain an enzymolysis material;
s3, adding a yeast fermentation culture medium into the enzymolysis material, inoculating the yeast after seed culture according to the inoculation amount of 2-5%, fermenting and culturing for 3-5 days, filtering, taking fermentation liquor, centrifuging, removing supernatant, and washing solid with distilled water for later use;
s4, adding activated carbon into the step S3, stirring and reacting for 1-2h, carrying out suction filtration by using a microporous filter membrane, and concentrating the filtrate to obtain the oligopeptide compound.
As a further improvement of the invention, the mass ratio of the whole chlamys farreri meat to the deep-sea fish scale in the step S1 is (2-5): 5; the mass volume ratio of the whole chlamys farreri meat to the distilled water is 1: (2-5) g/mL.
As a further improvement of the invention, in the step S2, the enzyme activities of the papain and the chymotrypsin are respectively 1000-1200U/g and 700-1000U/g, and the mass ratio is (1-3): 1.
as a further improvement of the invention, in the step S2, the enzymolysis condition is 37-40 ℃, the pH value is 5-7, the enzymolysis time is 5-8h, the enzyme deactivation condition is 100-120 ℃, and the enzyme deactivation time is 10-20 min.
As a further improvement of the invention, in step S3, the yeast is candida utilis; the yeast fermentation medium comprises the following components: 10-14g/L of glucose, 3-7g/L of sucrose, 8-10g/L, NaCl 3-7g/L of peptone and 2-5g/L, KH of ammonium nitrate2P04 0.5-2g/L、MgSO4﹒7H2O0.2-0.4 g/L and pH 5.5-5.7.
As a further improvement of the invention, the fermentation culture conditions in the step S3 are that the temperature is 28-32 ℃, the rotating speed is 100-150r/min, and the ventilation volume is 4-7 VVm.
As a further improvement of the invention, the mass ratio of the enzymolysis material to the yeast fermentation medium in the step S3 is 10: (4-7).
The invention further protects an oligopeptide compound prepared by the preparation method.
The invention further provides anti-wrinkle repair emulsion which is characterized by containing 2-5wt% of the oligopeptide compound.
As a further improvement of the invention, the feed additive comprises the following components in percentage by mass: 1-3% of sorbitan laurate, 2-4% of glycerol, 1-2.5% of 1, 2-propylene glycol, 0.01-0.04% of EDTA disodium, 2-4% of glyceryl caprylate, 0.1-0.7% of sodium dihydrogen phosphate, 2-5% of the oligopeptide complex of claim 8, 101-3% of coenzyme Q, and the balance of purified water.
The invention has the following beneficial effects: blood vessels are not distributed in deep sea fish scales, pathological changes, pollution or harmful toxins contained in the fish bodies cannot be biologically transferred through the blood vessels, so that the deep sea fish scales are the safest source of collagen, and meanwhile, the biological structure of the fish scales is closer to the human body, so that collagen peptides extracted from the deep sea fish scales are easier to absorb by the human body. After mixing and enzymolysis of deep-sea fish scales and scallop meat, carrying out enzymolysis on proteins with complex structures into smaller proteins, short peptides and the like, further fermenting the smaller proteins generated by enzymolysis through yeast to generate oligopeptides so as to obtain an oligopeptide compound, and removing aromatic hydrocarbon through active carbon to obtain hydrophobic amino acid in the oligopeptide compound: the content of valine, leucine and isoleucine is relatively high, the valine, leucine and isoleucine have the function of removing free radicals, and meanwhile, hydrophobic amino acids in peptide segments in the oligopeptide contribute to forming hydrophobic tails at carboxyl terminals of the peptide segments, so that the solubility of the peptide in lipid is improved, and further the antioxidant capacity is improved;
coenzyme q10 added in the anti-wrinkle repair emulsion can regularly condition cells generating energy and can also be used for improving acne and sun aging, which are one of the most undesirable problems, and everyone wants to have a young face. Therefore, anti-aging is a constant pursuit of beauty consumers. Wrinkles usually appear only due to aging, but now, the wrinkles are more and more aged, and the lower head is rather popular with wrinkle men. It can be seen that the generation of wrinkles has no absolute relation with age, and is more originated from people's habits. Perhaps when the face of the person is young and tight, the wrinkles appear quietly. The more wrinkles, the older. More and more people are concerned about wrinkles in T-shaped areas, and how to fade the wrinkles and relieve the wrinkles becomes more and more important.
At present, a lot of products for promoting wrinkle removal and wrinkle resistance exist, but a lot of comfortable and good-effect optional products do not exist. Many products with anti-wrinkle and wrinkle-removing effects have only simple relieving effects, and cannot realize effective deep repair of skin, so that wrinkles cannot be faded and removed fundamentally. In addition, many existing care products have anti-wrinkle and wrinkle-removing effects, which are usually added to other care products, such as facial masks or isolation creams, etc., as auxiliary functions, wherein the main functions are moisturizing and sun-screening, while the anti-wrinkle and wrinkle-removing effects are more and more added as additional added effects, and the actually generated anti-wrinkle and wrinkle-removing effects are very slight. Moreover, in many existing products with anti-wrinkle and anti-wrinkle effects, such as facial masks or isolation creams, etc., essence and/or pigment, etc. are usually added, the compounds and heavy metals contained in the composition can remain on the skin to cause pollution damage to the skin, but the skin of people is easy to age, the 1, 2-propylene glycol is not beneficial to improving the skin, has strong permeability, can help other components to be spread on the surface of the skin and permeate into the deep layer of the skin, but a small amount of diethylene glycol serving as a byproduct is mixed in the preparation process of propylene glycol, and tests show that the skin irritation of a 1, 2-propylene glycol and 1, 2-propylene glycol + coenzyme q10+ oligopeptide compound group shows that the latter shows low-sensitivity characteristics, and shows that the problem of large irritation caused by single 1, 2-propylene glycol is overcome after the combination of the three.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Deep sea fish scales are purchased from Baojie biological products limited company in Yangmen city, Jiangmen, Guangdong province; the chlamys farreri is purchased from the tobacco bench fishery Hongli aquatic product market.
Example 1
This example provides a method for preparing an oligopeptide complex, comprising the following steps:
s1, cleaning 20g of whole chlamys farreri meat, adding 40mL of distilled water, and grinding and homogenizing by a tissue triturator at 10000r/min to obtain slurry; then, 50g of deep sea fish scales are cleaned and crushed to obtain fish scale powder; uniformly mixing the fish scale powder and the slurry for later use;
s2, adding 1wt% of papain (with enzyme activity of 1000U/g) and 1wt% of chymotrypsin (with enzyme activity of 700U/g) in the feed liquid obtained in the step S1 into the feed liquid obtained in the step S1 respectively, and carrying out enzymolysis under the conditions of 37 ℃, pH 5, 5h and enzyme deactivation for 10min at the temperature of 100 ℃ to obtain an enzymolysis material;
s3, adding 40g of yeast fermentation culture medium into 100g of enzymolysis material, inoculating 2% of inoculation amount of candida utilis subjected to seed culture, performing fermentation culture under the conditions that the temperature is 28 ℃, the rotating speed is 100r/min and the ventilation volume is 4VVm, filtering after 3 days, taking fermentation liquor, centrifuging, removing supernatant, and washing solid with distilled water for later use;
the yeast fermentation medium comprises the following components: 10g/L glucose, 3g/L sucrose, 8g/L, NaCl 3g/L peptone and 2g/L, KH ammonium nitrate2P04 0.5g/L、MgSO4﹒7H2O is 0.2g/L, and the pH value is 5.5;
s4, adding 10g of activated carbon into the step S3, stirring and reacting for 1h, carrying out suction filtration by using a 0.45-micron microporous filter membrane, and concentrating the filtrate to obtain the oligopeptide compound.
Example 2
This example provides a method for preparing an oligopeptide complex, comprising the following steps:
s1, cleaning 50g of chlamys farreri whole meat, adding 250mL of distilled water, and grinding and homogenizing by a tissue triturator at 10000r/min to obtain slurry; then, 50g of deep sea fish scales are cleaned and crushed to obtain fish scale powder; uniformly mixing the fish scale powder and the slurry for later use;
s2, adding papain (with the enzyme activity of 1200U/g) accounting for 3wt% of the feed liquid in the step S1 and chymotrypsin (with the enzyme activity of 1000U/g) accounting for 1wt% of the feed liquid in the step S1 respectively, and carrying out enzymolysis under the conditions of 40 ℃, pH 7, 8h and enzyme deactivation for 20min at 120 ℃ to obtain an enzymolysis material;
s3, adding 70g of yeast fermentation culture medium into 100g of enzymolysis material, inoculating the candida utilis subjected to seed culture according to the inoculation amount of 5%, performing fermentation culture under the conditions that the temperature is 32 ℃, the rotating speed is 150r/min and the ventilation volume is 7VVm, filtering after 5 days, taking fermentation liquor, centrifuging, removing supernatant, and washing solid with distilled water for later use;
set of the yeast fermentation MediumThe method comprises the following steps: 14g/L glucose, 7g/L sucrose, 10g/L, NaCl 7g/L peptone and 2-5g/L, KH ammonium nitrate2P04 2g/L、MgSO4﹒7H2O0.4 g/L, pH 5.7;
s4, adding 10g of activated carbon into the step S3, stirring and reacting for 2 hours, carrying out suction filtration by using a 0.45-micron microporous filter membrane, and concentrating the filtrate to obtain the oligopeptide compound.
Example 3
This example provides a method for preparing an oligopeptide complex, comprising the following steps:
s1, washing 35g of chlamys farreri whole meat, adding 140mL of distilled water, and grinding and homogenizing by a tissue triturator at 10000r/min to obtain slurry; then, 50g of deep sea fish scales are cleaned and crushed to obtain fish scale powder; uniformly mixing the fish scale powder and the slurry for later use;
s2, adding 2wt% of papain (with the enzyme activity of 1100U/g) and 1wt% of chymotrypsin (with the enzyme activity of 800U/g) in the feed liquid obtained in the step S1 into the step S1 respectively, and carrying out enzymolysis under the conditions of 38 ℃, pH 6, 7h, enzyme deactivation under the conditions of 110 ℃ and 15min to obtain an enzymolysis material;
s3, adding 55g of yeast fermentation culture medium into 100g of enzymolysis material, inoculating the candida utilis subjected to seed culture according to the inoculation amount of 3.5%, performing fermentation culture under the conditions that the temperature is 30 ℃, the rotating speed is 125r/min and the ventilation volume is 5VVm, filtering after 4 days, taking fermentation liquor, centrifuging, removing supernatant, and washing solid with distilled water for later use;
the yeast fermentation medium comprises the following components: 12g/L glucose, 5g/L sucrose, 9g/L, NaCl 5g/L peptone and 3.5g/L, KH ammonium nitrate2P04 1g/L、MgSO4﹒7H2O is 0.3g/L, and the pH value is 5.6;
s4, adding 10g of activated carbon into the step S3, stirring and reacting for 1.5h, carrying out suction filtration by using a 0.45-micron microporous membrane, and concentrating the filtrate to obtain the oligopeptide compound.
Comparative example 1
Compared with the example 3, the deep sea fish scales are not added, and other conditions are not changed.
The method comprises the following steps:
s1, cleaning 85g of whole chlamys farreri meat, adding 340mL of distilled water, and grinding and homogenizing by a tissue triturator at 10000r/min to obtain slurry for later use;
s2, adding 2wt% of papain (with the enzyme activity of 1100U/g) and 1wt% of chymotrypsin (with the enzyme activity of 800U/g) in the feed liquid obtained in the step S1 into the step S1 respectively, and carrying out enzymolysis under the conditions of 38 ℃, pH 6, 7h, enzyme deactivation under the conditions of 110 ℃ and 15min to obtain an enzymolysis material;
s3, adding 55g of yeast fermentation culture medium into 100g of enzymolysis material, inoculating the candida utilis subjected to seed culture according to the inoculation amount of 3.5%, performing fermentation culture under the conditions that the temperature is 30 ℃, the rotating speed is 125r/min and the ventilation volume is 5VVm, filtering after 4 days, taking fermentation liquor, centrifuging, removing supernatant, and washing solid with distilled water for later use;
the yeast fermentation medium comprises the following components: 12g/L glucose, 5g/L sucrose, 9g/L, NaCl 5g/L peptone and 3.5g/L, KH ammonium nitrate2P04 1g/L、MgSO4﹒7H2O is 0.3g/L, and the pH value is 5.6;
s4, adding 10g of activated carbon into the step S3, stirring and reacting for 1.5h, carrying out suction filtration by using a 0.45-micron microporous membrane, and concentrating the filtrate to obtain the oligopeptide compound.
Comparative example 2
Compared with example 3, the whole chlamys farreri meat was not added, and other conditions were not changed.
The method comprises the following steps:
s1, cleaning and crushing 85g of deep sea fish scales to obtain fish scale powder, and mixing the fish scale powder with 140mL of water for later use;
s2, adding 2wt% of papain (with the enzyme activity of 1100U/g) and 1wt% of chymotrypsin (with the enzyme activity of 800U/g) in the feed liquid obtained in the step S1 into the step S1 respectively, and carrying out enzymolysis under the conditions of 38 ℃, pH 6, 7h, enzyme deactivation under the conditions of 110 ℃ and 15min to obtain an enzymolysis material;
s3, adding 55g of yeast fermentation culture medium into 100g of enzymolysis material, inoculating the candida utilis subjected to seed culture according to the inoculation amount of 3.5%, performing fermentation culture under the conditions that the temperature is 30 ℃, the rotating speed is 125r/min and the ventilation volume is 5VVm, filtering after 4 days, taking fermentation liquor, centrifuging, removing supernatant, and washing solid with distilled water for later use;
the yeast fermentation medium comprises the following components: 12g/L glucose, 5g/L sucrose, 9g/L, NaCl 5g/L peptone and 3.5g/L, KH ammonium nitrate2P04 1g/L、MgSO4﹒7H2O is 0.3g/L, and the pH value is 5.6;
s4, adding 10g of activated carbon into the step S3, stirring and reacting for 1.5h, carrying out suction filtration by using a 0.45-micron microporous membrane, and concentrating the filtrate to obtain the oligopeptide compound.
Comparative example 3
Compared with example 3, papain was not added, and other conditions were not changed.
The method comprises the following steps:
s1, washing 35g of chlamys farreri whole meat, adding 140mL of distilled water, and grinding and homogenizing by a tissue triturator at 10000r/min to obtain slurry; then, 50g of deep sea fish scales are cleaned and crushed to obtain fish scale powder; uniformly mixing the fish scale powder and the slurry for later use;
s2, adding chymotrypsin (with the enzyme activity of 800U/g) which accounts for 3wt% of the feed liquid in the step S1 into the step S1 respectively, and carrying out enzymolysis under the conditions of 38 ℃, pH 6, 7h and 110 ℃ for 15min to obtain an enzymolysis material;
s3, adding 55g of yeast fermentation culture medium into 100g of enzymolysis material, inoculating the candida utilis subjected to seed culture according to the inoculation amount of 3.5%, performing fermentation culture under the conditions that the temperature is 30 ℃, the rotating speed is 125r/min and the ventilation volume is 5VVm, filtering after 4 days, taking fermentation liquor, centrifuging, removing supernatant, and washing solid with distilled water for later use;
the yeast fermentation medium comprises the following components: 12g/L glucose, 5g/L sucrose, 9g/L, NaCl 5g/L peptone and 3.5g/L, KH ammonium nitrate2P04 1g/L、MgSO4﹒7H2O is 0.3g/L, and the pH value is 5.6;
s4, adding 10g of activated carbon into the step S3, stirring and reacting for 1.5h, carrying out suction filtration by using a 0.45-micron microporous membrane, and concentrating the filtrate to obtain the oligopeptide compound.
Comparative example 4
Compared with example 3, chymotrypsin was not added, and other conditions were not changed.
The method comprises the following steps:
s1, washing 35g of chlamys farreri whole meat, adding 140mL of distilled water, and grinding and homogenizing by a tissue triturator at 10000r/min to obtain slurry; then, 50g of deep sea fish scales are cleaned and crushed to obtain fish scale powder; uniformly mixing the fish scale powder and the slurry for later use;
s2, adding papain (with the enzyme activity of 1100U/g) accounting for 3wt% of the feed liquid in the step S1 into the step S1 respectively, and carrying out enzymolysis under the conditions of 38 ℃, pH 6 and 7h, and carrying out enzyme deactivation under the conditions of 110 ℃ and 15min to obtain an enzymolysis material;
s3, adding 55g of yeast fermentation culture medium into 100g of enzymolysis material, inoculating the candida utilis subjected to seed culture according to the inoculation amount of 3.5%, performing fermentation culture under the conditions that the temperature is 30 ℃, the rotating speed is 125r/min and the ventilation volume is 5VVm, filtering after 4 days, taking fermentation liquor, centrifuging, removing supernatant, and washing solid with distilled water for later use;
the yeast fermentation medium comprises the following components: 12g/L glucose, 5g/L sucrose, 9g/L, NaCl 5g/L peptone and 3.5g/L, KH ammonium nitrate2P04 1g/L、MgSO4﹒7H2O is 0.3g/L, and the pH value is 5.6;
s4, adding 10g of activated carbon into the step S3, stirring and reacting for 1.5h, carrying out suction filtration by using a 0.45-micron microporous membrane, and concentrating the filtrate to obtain the oligopeptide compound.
Comparative example 5
Compared with the example 3, the step of S2 enzymolysis is not carried out, and other conditions are not changed.
This example provides a method for preparing an oligopeptide complex, comprising the following steps:
s1, washing 35g of chlamys farreri whole meat, adding 140mL of distilled water, and grinding and homogenizing by a tissue triturator at 10000r/min to obtain slurry; then, 50g of deep sea fish scales are cleaned and crushed to obtain fish scale powder; uniformly mixing the fish scale powder and the slurry for later use;
s2, adding 55g of yeast fermentation medium into 100g of the material obtained in the step S1, inoculating the Candida utilis subjected to seed culture according to the inoculation amount of 3.5%, performing fermentation culture under the conditions that the temperature is 30 ℃, the rotating speed is 125r/min, the ventilation amount is 5VVm, filtering after 4 days, taking fermentation liquor, centrifuging, removing supernatant, and washing solid with distilled water for later use;
the yeast fermentation medium comprises the following components: 12g/L glucose, 5g/L sucrose, 9g/L, NaCl 5g/L peptone and 3.5g/L, KH ammonium nitrate2P04 1g/L、MgSO4﹒7H2O is 0.3g/L, and the pH value is 5.6;
s3, adding 10g of activated carbon into the step S2, stirring and reacting for 1.5h, carrying out suction filtration by using a 0.45-micron microporous filter membrane, and concentrating the filtrate to obtain the oligopeptide compound.
Comparative example 6
Compared with example 3, the fermentation step of step S3 was not performed, and other conditions were not changed.
This example provides a method for preparing an oligopeptide complex, comprising the following steps:
s1, washing 35g of chlamys farreri whole meat, adding 140mL of distilled water, and grinding and homogenizing by a tissue triturator at 10000r/min to obtain slurry; then, 50g of deep sea fish scales are cleaned and crushed to obtain fish scale powder; uniformly mixing the fish scale powder and the slurry for later use;
s2, adding 2wt% of papain (with the enzyme activity of 1100U/g) and 1wt% of chymotrypsin (with the enzyme activity of 800U/g) in the feed liquid obtained in the step S1 into the step S1 respectively, and carrying out enzymolysis under the conditions of 38 ℃, pH 6, 7h, enzyme deactivation under the conditions of 110 ℃ and 15min to obtain an enzymolysis material;
s2, adding 10g of activated carbon into the enzymolysis material in the step S2, stirring and reacting for 1.5h, carrying out suction filtration by using a 0.45-micron microporous filter membrane, and concentrating the filtrate to obtain the oligopeptide compound.
Example 4 anti-wrinkle repair emulsion
The composition comprises the following components in percentage by mass: sorbitan laurate 1%, glycerol 2%, 1, 2-propanediol 1%, disodium EDTA 0.01%, glyceryl caprylate 2%, sodium dihydrogen phosphate 0.1%, oligopeptide complex prepared in example 1 2%, coenzyme Q101%, and the balance purified water.
The preparation method comprises the following steps:
1) adding purified water of formula amount into water phase pot, slowly adding 1, 2-propylene glycol, glycerol, sodium dihydrogen phosphate, oligopeptide compound and EDTA disodium under stirring, heating to 75 deg.C, stirring, and keeping the temperature for 3 min;
2) adding sorbitan laurate, glyceryl caprylate and coenzyme Q10 into an oil phase pot according to the formula amount, heating to 75 ℃, uniformly stirring, and keeping the temperature for 5 min;
3) filtering the materials in the water phase and oil phase pot, sequentially pumping into a vacuum emulsifying pot, homogenizing for 5min, slowly cooling to 40 deg.C, stirring, testing, discharging, and bottling.
Example 5 anti-wrinkle repair emulsion
Compared with the example 4, the formula components are different, and the preparation method is consistent.
The composition comprises the following components in percentage by mass: 3% of sorbitan laurate, 4% of glycerol, 2.5% of 1, 2-propylene glycol, 0.04% of disodium EDTA, 4% of caprylic acid glycerol, 0.7% of sodium dihydrogen phosphate, 5% of the oligopeptide complex prepared in example 2, 103% of coenzyme Q, and the balance of purified water.
Example 6 anti-wrinkle repair emulsion
Compared with the example 4, the formula and the components are different, and the preparation method is consistent.
The composition comprises the following components in percentage by mass: sorbitan laurate 2%, glycerol 3%, 1, 2-propanediol 1-2.5%, disodium EDTA 0.02%, glyceryl caprylate 3%, sodium dihydrogen phosphate 0.5%, oligopeptide complex 3.5% prepared in example 3, coenzyme Q102%, and the balance purified water.
Comparative example 7
Compared with example 6, coenzyme Q10 was not added, and other conditions were not changed.
The composition comprises the following components in percentage by mass: sorbitan laurate 2%, glycerol 3%, 1, 2-propanediol 1-2.5%, disodium EDTA 0.02%, glyceryl caprylate 3%, sodium dihydrogen phosphate 0.5%, 5.5% oligopeptide complex prepared in example 3, and the balance purified water.
Comparative example 8
In comparison with example 6, the oligopeptide complex prepared in example 3 was not added, and other conditions were not changed.
The composition comprises the following components in percentage by mass: 2% of sorbitan laurate, 3% of glycerol, 1-2.5% of 1, 2-propylene glycol, 0.02% of EDTA disodium, 3% of glyceryl caprylate, 0.5% of sodium dihydrogen phosphate, 105.5% of coenzyme Q, and the balance of purified water.
Comparative example 9
Compared with example 6, the oligopeptide complex prepared in example 3 and coenzyme Q10 were not added, and other conditions were not changed.
Comparative example 10
Compared with example 6, the oligopeptide complex prepared in example 3 is replaced by the oligopeptide complex prepared in comparative example 1, and other conditions are not changed.
Comparative example 11
Compared with example 6, the oligopeptide complex prepared in example 3 is replaced by the oligopeptide complex prepared in comparative example 2, and other conditions are not changed.
Comparative example 12
Compared with example 6, the oligopeptide complex prepared in example 3 is replaced by the oligopeptide complex prepared in comparative example 3, and other conditions are not changed.
Comparative example 13
Compared with example 6, the oligopeptide complex prepared in example 3 is replaced by the oligopeptide complex prepared in comparative example 4, and other conditions are not changed.
Comparative example 14
Compared with example 6, the oligopeptide complex prepared in example 3 was replaced by the oligopeptide complex prepared in comparative example 5, and other conditions were not changed.
Comparative example 15
Compared with example 6, the oligopeptide complex prepared in example 3 is replaced by the oligopeptide complex prepared in comparative example 6, and other conditions are not changed.
Test example 1 Patch test
360 volunteers of 20-48 years old who meet the test requirements are selected as the test subjects, the test subjects are randomly divided into 8 groups, 30 volunteers are selected in each group, according to the skin closed patch test of the human skin patch test in the technical Specification for cosmetic safety, whether the products of examples 4-6 and comparative examples 7-15 have the potential possibility of causing adverse reaction to human bodies, the results are interpreted according to the interpretation standards in the following Table 1, and the statistical interpretation results are shown in the following Table 2.
TABLE 1
Figure 351864DEST_PATH_IMAGE002
TABLE 2
Figure 990043DEST_PATH_IMAGE004
The patch test shows that examples 4-6 and comparative examples 10-15 of the present invention have low sensitivity, no coenzyme Q10 is added in comparative example 7, no oligopeptide complex is added in comparative example 8, suspicious and positive reactions occur, no coenzyme Q10 and oligopeptide complex are added in comparative example 9, and even strong positive reactions occur, and as can be seen from the results of examples 6 and comparative examples 7-9, 1, 2-propanediol alone has strong anaphylaxis, and the combination of 1, 2-propanediol + coenzyme Q10+ oligopeptide complex overcomes the problem of large irritation caused by the single use of 1, 2-propanediol alone.
Test example 2
Skin texture measurements were performed using the products of examples 4-6 of the present invention and comparative examples 7-15, respectively. Firstly, 120 female testees with healthy skin are selected, the left half face of the testee is coated with the toning lotion prepared by the invention to serve as an experimental group, and the other half face of the testee is not coated with any substance to serve as a blank group. The experiment is 8 weeks, the skin of the testee is detected and analyzed by various instruments at 1 week, 4 weeks and 8 weeks respectively, the improvement effects of the toning lotion on the moisture content of the skin, the elasticity of the skin, fine wrinkles, the roughness of the skin, the sebum secretion amount and the number of coarse and large pores are evaluated, and the average values of the three tests at 1 week, 4 week and 8 week are shown in table 3.
TABLE 3
Figure 363256DEST_PATH_IMAGE006
Note: "+" is increasing and "-" is decreasing.
The results show (see table 2) that the hair product has different degrees of reduction on the number of fine lines, roughness, sebum secretion and coarse pores of the skin, has obvious effect of improving the moisture content and the elasticity of the skin, and shows that the hair product has the effect of improving the skin quality of the skin.
Compared with the example 6, the coenzyme Q10 is not added in the comparative example 7, the effects of improving the skin elasticity and the skin roughness and reducing fine wrinkles and the like are obviously reduced, and the coenzyme Q10 can regularly condition cells generating energy and can also be used for improving pimples and sun damage;
compared with the example 6, the comparative example 8 has no oligopeptide compound, so that the effects of reducing fine wrinkles, keeping skin moisture, improving skin elasticity, refining pores and the like are obviously reduced; and (3) removing aromatic hydrocarbon from the oligopeptide compound through active carbon, wherein the hydrophobic amino acid: the content of valine, leucine and isoleucine is relatively high, the valine, leucine and isoleucine have the function of removing free radicals, and meanwhile, hydrophobic amino acids in peptide segments in the oligopeptide contribute to forming hydrophobic tails at carboxyl terminals of the peptide segments, so that the solubility of the peptide in lipid is improved, and further the antioxidant capacity is improved;
compared with the example 6, the coenzyme Q10 and the oligopeptide compound are not added in the comparative example 9, so that the reduction degree of fine lines, roughness, sebum secretion and coarse and large pore number of the skin is obviously reduced, the improvement rate of the moisture content and the elasticity of the skin is not high, and the obvious effect is hardly realized, therefore, under the synergistic effect of the coenzyme Q10 and the oligopeptide compound, the damaged cells can be obviously repaired, the fine lines can be smoothed, and the obvious effects of resisting wrinkles and ageing are realized.
Compared with the example 6, the comparative example 10 and the comparative example 11 are respectively not added with deep sea fish scales or chlamys farreri full meat during the preparation of the oligopeptide compound, the effects of improving skin elasticity and weakening fine lines are obviously reduced in the comparative example 10, the effects of improving skin roughness, inhibiting sebum secretion and refining pores are obviously reduced in the comparative example 11, different raw materials can be seen, the skin improvement effects are different, the two are mixed and compounded, a product with excellent comprehensive skin improvement effect can be prepared, and the compounding has obvious synergy.
Compared with the example 6, the comparative examples 12 and 13 have the advantages that the papain or chymotrypsin is not added in the preparation of the oligopeptide compound, and the enzymolysis effect on the substrate is not as good as that of the compound enzyme due to the addition of only a single protease, so that the skin improvement effect on the prepared product is reduced.
Comparative example 14 and comparative example 15 compared with example 6, in which the oligopeptide complex was prepared without enzymatic hydrolysis or fermentation, respectively, the hydrolytic fermentation effect on the fish scale powder and the homogenate substrate was poor, resulting in a certain reduction in the index.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (10)

1. The preparation method of the oligopeptide compound is characterized by comprising the following steps:
s1, cleaning the whole chlamys farreri meat, adding distilled water, and homogenizing to obtain slurry; then, cleaning and crushing deep sea fish scales to obtain fish scale powder; uniformly mixing the fish scale powder and the slurry for later use;
s2, adding papain and chymotrypsin in the step S1, performing enzymolysis, and inactivating enzyme to obtain an enzymolysis material;
s3, adding a yeast fermentation culture medium into the enzymolysis material, inoculating the yeast after seed culture according to the inoculation amount of 2-5%, fermenting and culturing for 3-5 days, filtering, taking fermentation liquor, centrifuging, removing supernatant, and washing solid with distilled water for later use;
s4, adding activated carbon into the step S3, stirring and reacting for 1-2h, carrying out suction filtration by using a microporous filter membrane, and concentrating the filtrate to obtain the oligopeptide compound.
2. The method for preparing a chlamys farreri meat-fish scale of claim 1, wherein the mass ratio of the chlamys farreri whole meat to the deep-sea fish scale in step S1 is (2-5): 5; the mass volume ratio of the whole chlamys farreri meat to the distilled water is 1: (2-5) g/mL.
3. The preparation method according to claim 1, wherein the enzyme activities of the papain and the chymotrypsin in step S2 are 1000-1200U/g and 700-1000U/g respectively, and the mass ratio is (1-3): 1.
4. the method as claimed in claim 1, wherein the enzymolysis condition in step S2 is 37-40 ℃, pH is 5-7, enzymolysis time is 5-8h, enzyme deactivation condition is 100-120 ℃, and enzyme deactivation time is 10-20 min.
5. The method according to claim 1, wherein the yeast in step S3 is candida utilis; the yeast fermentation medium comprises the following components: 10-14g/L of glucose, 3-7g/L of sucrose, 8-10g/L, NaCl 3-7g/L of peptone and 2-5g/L, KH of ammonium nitrate2P04 0.5-2g/L、MgSO4﹒7H2O0.2-0.4 g/L and pH 5.5-5.7.
6. The method as claimed in claim 1, wherein the fermentation conditions in step S3 are a temperature of 28-32 ℃, a rotation speed of 100-150r/min, and an aeration rate of 4-7 VVm.
7. The preparation method according to claim 1, wherein the mass ratio of the enzymolysis material to the yeast fermentation medium in the step S3 is 10: (4-7).
8. An oligopeptide complex prepared by the preparation method according to any one of claims 1 to 7.
9. An anti-wrinkle repair emulsion comprising 2 to 5wt% of the oligopeptide complex according to claim 8.
10. The anti-wrinkle repair emulsion according to claim 9, characterized in that it comprises the following components in mass fraction: 1-3% of sorbitan laurate, 2-4% of glycerol, 1-2.5% of 1, 2-propylene glycol, 0.01-0.04% of EDTA disodium, 2-4% of glyceryl caprylate, 0.1-0.7% of sodium dihydrogen phosphate, 2-5% of the oligopeptide complex of claim 8, 101-3% of coenzyme Q, and the balance of purified water.
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