CN112494361A - Antibacterial and anti-radiation marine oligosaccharide isolation emulsion and preparation method thereof - Google Patents

Antibacterial and anti-radiation marine oligosaccharide isolation emulsion and preparation method thereof Download PDF

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CN112494361A
CN112494361A CN202011576390.9A CN202011576390A CN112494361A CN 112494361 A CN112494361 A CN 112494361A CN 202011576390 A CN202011576390 A CN 202011576390A CN 112494361 A CN112494361 A CN 112494361A
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oligosaccharide
radiation
enzymolysis
carrageenan
antibacterial
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高芹芹
张斌
管昶
徐小龙
王丽丽
岳帆
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Qingdao Bz Oligo Biotech Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
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    • A61P31/00Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/02Local antiseptics
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/04Antibacterial agents
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61Q17/005Antimicrobial preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations

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Abstract

The invention discloses an antibacterial and anti-radiation marine oligosaccharide isolation emulsion and a preparation method thereof, brown alga oligosaccharides with the weight-average molecular weight of less than 20OODa, carrageenan oligosaccharides with the weight-average molecular weight of less than 2000Da and a mixture of the two in proportion are selected as natural isolation emulsion additives, the two oligosaccharides are combined under certain concentration to have strong antibacterial and anti-radiation effects, and the product using the two oligosaccharides in cosmetics has good antibacterial and anti-radiation effects. In addition, the pH regulator in the raw materials can regulate the pH value of the skin, so that the skin can be kept in the optimal state.

Description

Antibacterial and anti-radiation marine oligosaccharide isolation emulsion and preparation method thereof
Technical Field
The invention discloses an antibacterial and anti-radiation marine oligosaccharide isolation emulsion and a preparation method thereof, and particularly belongs to the technical field of marine organisms.
Background
With the continuous improvement of the material and cultural living standard of people and the development and progress of society, cosmetics become daily necessities for beautifying life of people. At present, beauty cosmetics are listed in ten major industries of the country in China, the safety of the cosmetics is almost the primary consideration for purchasing the cosmetics by all consumers, and organic, natural and non-additive products are necessary conditions for ensuring the safety of the products. The seaweed forms a specific metabolic mode in a long-term evolution process due to the specific living environment of the seaweed, generates a plurality of chemical components with specific physiological functions, such as sulfated polysaccharide, superoxide dismutase and the like, has various health-care functions, such as antioxidation, anti-inflammation sterilization, ultraviolet protection, anti-aging and the like, and is a natural and multifunctional bioactive additive. China has abundant seaweed resources, so that the preparation of cosmetics by taking the abundant seaweed resources as raw materials is a main direction of the cosmetic industry.
Atmospheric pollution and increasingly thin ozone layer cause that the number of patients suffering from solar dermatitis and skin cancer is obviously increased in the global range. Segregation is a constant theme of cosmetic development.
Algin is produced from kelp and kelp, and is a linear polymer composed of beta-D-polymannuronic acid (M) and alpha-L-polyguluronic acid (G), which is a natural polysaccharide. The molecular weight of the algin is reduced by applying modern marine biotechnology, the polymerization degree of algin sugar chain is controlled within 2-20 monosaccharides, and the algin oligosaccharide is prepared and has low molecular weight, the algin oligosaccharide has biocompatibility and water solubility, the alginate oligosaccharide has biological activities of moisture absorption and water retention, radiation resistance, ultraviolet resistance, oxidation resistance, free radical removal and aging resistance, effective heavy metal ion adsorption, effective bacteriostasis and the like, and is safe and nontoxic according to the activity principle of a daily chemical product such as an excellent cosmetic skin care product.
The carrageenan is a natural marine sulfated polysaccharide with a unique structure and is called heparan-like polysaccharide, and experimental research shows that the carrageenan has the biological activities of anti-angiogenesis, anti-tumor, immunoregulation, antioxidation, antibiosis, radiation resistance, antivirus, blood sugar reduction and the like. However, the application of carrageenan polysaccharide is limited due to the reasons of large molecular weight, poor solubility and absorptivity, complex structure and the like. The carrageenan oligosaccharide has the advantages of small molecular weight, enhanced solubility, simplified structure, easy absorption, increased stability and safety, fully exposed active groups after the polysaccharide chains are broken in different forms, obviously improved activity compared with the carrageenan, and low toxicity, so that the application range of the carrageenan is widened, and the research on the activity of the carrageenan oligosaccharide is increasingly concerned at present.
At present, although there are technical reports of applying alginate oligosaccharides and carrageenan oligosaccharides to cosmetics, the comprehensive utilization of alginate oligosaccharides and carrageenan oligosaccharides for preparing bacteriostatic and anti-radiation marine oligosaccharide isolation milk is only reported, and the application of marine oligosaccharides in cosmetics is also restrained.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the antibacterial and anti-radiation marine oligosaccharide isolation milk and the preparation method thereof, brown alga oligosaccharides with the weight-average molecular weight of less than 20OODa, carrageenan oligosaccharides with the weight-average molecular weight of less than 2000Da and a mixture of the two oligosaccharides in proportion are selected as natural isolation milk additives, the two oligosaccharides are combined under certain concentration to have strong antibacterial and anti-radiation effects, and the antibacterial and anti-radiation effects are good when the two oligosaccharides are used in cosmetics. In addition, the product selects marine oligosaccharide from oceans, and has the advantages of being green, safe and the like.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the invention provides an antibacterial and anti-radiation marine oligosaccharide isolation milk, which is characterized in that the formula of the marine oligosaccharide isolation milk is as follows:
water phase: 51.5 parts of deionized water, 0.2 part of alginate oligosaccharide, 0.2 part of carrageenan oligosaccharide and 5 parts of glycerol; adjusting the pH value to 5.6 by using citric acid;
oil phase: 2 parts of glycerol monostearate, 4 parts of dimethyl silicone oil, 1 part of octadecanol and 6 parts of olive oil;
auxiliary materials: 0.5 part of p-hydroxy-phenyl propionate, and a proper amount of essence and vitamin E.
The marine oligosaccharide isolation milk is prepared by the following steps:
heating and mixing the water phase in a 90 ℃ water bath for 15 minutes to fully dissolve the water phase, heating and mixing the oil phase in a 90 ℃ water bath for 15 minutes to fully dissolve the oil phase, then placing the mixture in a 65 ℃ constant temperature water bath, slowly adding the water phase, stirring the mixture uniformly, cooling to 50 ℃, adding auxiliary materials, homogenizing the mixture by using a homogenizer, and subpackaging the mixture to obtain the product.
The brown algae oligosaccharide is prepared by the following steps:
weighing sodium alginate, preparing into 1% water solution with distilled water, heating and stirring at 60 deg.C in a magnetic stirrer to dissolve completely; adding 10ml of alginate lyase into the dissolved alginate solution, and reacting for 12h at 60 ℃ on a magnetic stirrer; inactivating the liquid after enzymolysis at 100 ℃ for 15 min; performing high-speed centrifugation on the enzymolysis product at 8000r/min for 10 min; vacuum freeze-drying the enzymolysis liquid to obtain the brown algae oligosaccharide powder.
The molecular weight of the brown algae oligosaccharide is less than 2000 Da.
The carrageenan oligosaccharide is prepared by the following steps:
weighing carrageenan raw material, and adding 0.1mol/L Na2HPO4·12H2O is prepared into a solution with the concentration of 1 percent, and the solution is heated and stirred at 40 ℃ to be completely dissolved; mixing the carrageenin enzymolysis solution and the dissolved carrageenin solution according to the proportion of 1:7-10, heating in water bath at 40 ℃ and stirring for 5-10 min; inactivating the liquid after enzymolysis at 100 ℃ for 15 min; performing high-speed centrifugation on the enzymolysis product at 8000r/min for 10 min; and (4) carrying out vacuum freeze drying on the enzymolysis liquid to obtain carrageenan oligosaccharide powder.
The molecular weight of the carrageenan oligose is less than 2000 Da.
The carrageenan enzymolysis liquid is prepared by the following steps:
inoculating the screened Cellulophagalytica strain N5-2 into an activation culture medium, performing shake culture at 20-30 ℃ and 250rpm/min for 15-20h, and performing culture activation; inoculating the seed liquid into a fermentation culture medium according to the inoculation amount of 2-4%, and performing shake cultivation at 20-30 ℃ and 150-250rpm/min for 15-20 h; freezing and centrifuging the fermentation liquor at the temperature of 4 ℃ for 20min at 4000-.
The invention provides an antibacterial and anti-radiation marine oligosaccharide isolation emulsion and a preparation method thereof, and the emulsion has the following beneficial effects: according to the invention, the brown algae oligosaccharide and the carrageenan oligosaccharide are combined under a certain concentration to have a strong antibacterial and anti-radiation effect, and the product using the brown algae oligosaccharide and the carrageenan oligosaccharide has a good antibacterial and anti-radiation effect. The carrageenan oligosaccharide has an obvious protective effect on radiation damage, has strong activity of eliminating superoxide anion free radicals and light free radicals, and has reducing capacity, the brown alga oligosaccharide also has antioxidant activity, the carrageenan oligosaccharide and the brown alga oligosaccharide are matched with each other, the antioxidant activity is enhanced, and further the damaged skin can be repaired.
Drawings
FIG. 1: inhibiting effect of different isolations on Escherichia coli;
FIG. 2: inhibition of staphylococcus aureus by different barrier milks.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be illustrative, not limiting and are not intended to limit the scope of the invention.
Example 1
An antibacterial and anti-radiation marine oligosaccharide isolation emulsion comprises the following formula:
water phase: 51.5 parts of deionized water, 0.2 part of alginate oligosaccharide, 0.2 part of carrageenan oligosaccharide and 5 parts of glycerol; adjusting the pH value to 5.6 by using citric acid;
oil phase: 2 parts of glycerol monostearate, 4 parts of dimethyl silicone oil, 1 part of octadecanol and 6 parts of olive oil;
auxiliary materials: 0.5 part of p-hydroxy-phenyl propionate, and proper amount of essence and vitamin E;
the marine oligosaccharide isolation milk is prepared by the following steps: heating and mixing the water phase in a 90 ℃ water bath kettle for 15 minutes to fully dissolve the water phase, heating and mixing the oil phase in the 90 ℃ water bath kettle for 15 minutes to fully dissolve the oil phase, then placing the mixture in a 65 ℃ constant temperature water bath, slowly adding the water phase, stirring uniformly, cooling to 50 ℃, adding auxiliary materials, homogenizing by using a homogenizer, and subpackaging to obtain a product;
the brown algae oligosaccharide is prepared by the following steps: weighing sodium alginate, preparing into 1% water solution with distilled water, heating and stirring at 60 deg.C in a magnetic stirrer to dissolve completely; adding 10ml of alginate lyase into the dissolved alginate solution, and reacting for 12h at 60 ℃ on a magnetic stirrer; inactivating the liquid after enzymolysis at 100 ℃ for 15 min; performing high-speed centrifugation on the enzymolysis product at 8000r/min for 10 min; vacuum freeze-drying the enzymolysis liquid to obtain brown algae oligosaccharide powder;
the carrageenan oligosaccharide is prepared by the following steps: weighing carrageenan raw material, and adding 0.1mol/L Na2HPO4·12H2O is prepared into a solution with the concentration of 1 percent, and the solution is heated and stirred at 40 ℃ to be completely dissolved; mixing the carrageenin enzymolysis solution and the dissolved carrageenin solution according to the proportion of 1:7-10, heating in water bath at 40 ℃ and stirring for 5-10 min; inactivating the liquid after enzymolysis at 100 ℃ for 15 min; performing high-speed centrifugation on the enzymolysis product at 8000r/min for 10 min; vacuum freeze drying the enzymolysis liquid to obtain carrageenan oligose powder;
the carrageenan enzymolysis liquid is prepared by the following steps: inoculating the screened Cellulophagalytica strain N5-2 into an activation culture medium, performing shake culture at 20-30 ℃ and 250rpm/min for 15-20h, and performing culture activation; inoculating the seed liquid into a fermentation culture medium according to the inoculation amount of 2-4%, and performing shake cultivation at 20-30 ℃ and 150-250rpm/min for 15-20 h; freezing and centrifuging the fermentation liquor at the temperature of 4 ℃ for 20min at 4000-.
Example 2 Natural Marine oligosaccharide isolation milk bacteriostasis experiment
Respectively inoculating the culture solution of Escherichia coli broth cultured overnight into 3 groups of broth culture solutions without addition of isolation milk, common bacteriostatic agent emulsion and marine oligosaccharide emulsion at a ratio of 2%, shaking up each group of culture solution, and subpackaging into 11 sterile test tubes with 5 mL each. The tubes in each group were subjected to shake cultivation at 37 ℃ and 1 tube was taken out from each group at 0,1,2,3,4,5,6,7,8,9,10 h, and the OD600 was measured and recorded, and the OD600 was plotted as ordinate and the cultivation time as abscissa, to plot the growth curve (Shennu et al, 1999); the experimental results are shown in fig. 1 and fig. 2;
as can be seen from figures 1 and 2, the culture medium containing marine oligosaccharide has certain inhibition effect on the growth of escherichia coli and staphylococcus aureus, and is superior to the inhibition effect of the isolation milk of the common bacteriostatic agent.
Example 3 Marine oligosaccharide isolation emulsion antiradiation test
Body mass (20. + -.2) g of clean grade male mice 40 were removed from the dorsal coat with 8% sodium sulfide only 2 days prior to the test and exposed to an area of 4cmX3 cm. 2d after depilation, mice were randomly divided into a positive control group (10), a blank control group (10), a model group (10) and a test group (10);
a commercial sun screen is applied to a positive control group, a moisturizer prepared from no active ingredient is applied to a blank control group and a model group, a sun screen prepared from an active ingredient (marine oligosaccharide) is applied to a test group, 0.3g of sun screen is applied to each back, 0.1g of sun screen is applied to each ear, and the ratio of sun screen to sun screen is 2 times/d, and the sun screen is applied for 3 days. Except for the blank control group, the mice in other groups are horizontally fixed, are vertically spaced from an ultraviolet lamp by 15 cm, are irradiated for 6 hours, and protect the eyes of the animals from ultraviolet radiation injury during the irradiation period to form a skin damage mouse model. Continuously irradiating the skin damage mouse model with ultraviolet rays for 40h, killing the mouse, weighing and recording the mass of the mouse body, then respectively taking two ears and a circular ear piece and a skin piece with the diameter of 9mm at the back, accurately weighing the ear mass and the cortex quantity, and calculating an ear index and a skin index, wherein the ear index = ear mass/body mass and the skin index = skin mass/body mass;
TABLE 1 test results of ear index and skin index of ultraviolet mice
Figure DEST_PATH_IMAGE002
As can be seen from Table 1, the ear and skin indexes of the model group are higher than those of the blank group and are all significant differences (P <0.O1) compared with those of the blank group, the ear and skin indexes of the test group are lower than those of the model group and are all significant differences (P <0. O5S) compared with those of the model group, and the ear and skin indexes of the positive control group are lower than those of the model group compared with those of the model group, and the ear indexes are not significant differences and the skin indexes are significant differences (P <0. O1). The data show that the marine oligosaccharide isolation emulsion has better ultraviolet protection effect on mice than common commercial isolation creams. The marine oligosaccharide isolation milk can play an obvious ultraviolet protection role in a mouse test.
The above embodiments are only used for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof; such modifications and substitutions do not depart from the spirit and scope of the present invention as set forth in the appended claims.

Claims (7)

1. An antibacterial and anti-radiation marine oligosaccharide isolation emulsion is characterized in that the formula of the marine oligosaccharide isolation emulsion is as follows:
water phase: 51.5 parts of deionized water, 0.2 part of alginate oligosaccharide, 0.2 part of carrageenan oligosaccharide and 5 parts of glycerol; adjusting the pH value to 5.6 by using citric acid;
oil phase: 2 parts of glycerol monostearate, 4 parts of dimethyl silicone oil, 1 part of octadecanol and 6 parts of olive oil;
auxiliary materials: 0.5 part of p-hydroxy-phenyl propionate, and a proper amount of essence and vitamin E.
2. The bacteriostatic radiation-resistant marine oligosaccharide isolation milk according to claim 1, which is prepared by the following steps:
heating and mixing the water phase in a 90 ℃ water bath for 15 minutes to fully dissolve the water phase, heating and mixing the oil phase in a 90 ℃ water bath for 15 minutes to fully dissolve the oil phase, then placing the mixture in a 65 ℃ constant temperature water bath, slowly adding the water phase, stirring the mixture uniformly, cooling to 50 ℃, adding auxiliary materials, homogenizing the mixture by using a homogenizer, and subpackaging the mixture to obtain the product.
3. The antibacterial and anti-radiation marine oligosaccharide isolation milk as claimed in claim 1, characterized in that the brown algae oligosaccharide is prepared by the following steps:
weighing sodium alginate, preparing into 1% water solution with distilled water, heating and stirring at 60 deg.C in a magnetic stirrer to dissolve completely; adding 10ml of alginate lyase into the dissolved alginate solution, and reacting for 12h at 60 ℃ on a magnetic stirrer; inactivating the liquid after enzymolysis at 100 ℃ for 15 min; performing high-speed centrifugation on the enzymolysis product at 8000r/min for 10 min; vacuum freeze-drying the enzymolysis liquid to obtain the brown algae oligosaccharide powder.
4. The bacteriostatic radiation-resistant marine oligosaccharide isolation milk according to claim 1, characterized in that the molecular weight of the brown algae oligosaccharide is less than 2000 Da.
5. The antibacterial anti-radiation marine oligosaccharide isolation milk according to claim 1, characterized in that the carrageenan oligosaccharide is prepared by the following steps:
weighing carrageenan raw material, and adding 0.1mol/L Na2HPO4·12H2O is prepared into a solution with the concentration of 1 percent, and the solution is heated and stirred at 40 ℃ to be completely dissolved; mixing the carrageenin enzymolysis solution and the dissolved carrageenin solution according to the proportion of 1:7-10, heating in water bath at 40 ℃ and stirring for 5-10 min; inactivating the liquid after enzymolysis at 100 ℃ for 15 min; performing high-speed centrifugation on the enzymolysis product at 8000r/min for 10 min; vacuum freeze drying the enzymolysis liquid to obtain the cardLargol oligosaccharide powder.
6. The bacteriostatic radiation-resistant marine oligosaccharide isolation milk according to claim 1, characterized in that the molecular weight of the carrageenan oligosaccharide is less than 2000 Da.
7. The antibacterial and anti-radiation marine oligosaccharide isolation emulsion as claimed in claim 5, wherein the carrageenan enzymolysis solution is prepared by the following steps:
inoculating the screened Cellulophagalytica strain N5-2 into an activation culture medium, performing shake culture at 20-30 ℃ and 250rpm/min for 15-20h, and performing culture activation; inoculating the seed liquid into a fermentation culture medium according to the inoculation amount of 2-4%, and performing shake cultivation at 20-30 ℃ and 150-250rpm/min for 15-20 h; freezing and centrifuging the fermentation liquor at the temperature of 4 ℃ for 20min at 4000-.
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CN114903813A (en) * 2022-04-19 2022-08-16 青岛和海生物科技有限公司 Emulsion added with marine oligosaccharide composition for preventing and relieving chapped skin
CN115089502A (en) * 2022-08-15 2022-09-23 李瑶 Moisturizing essence milk and preparation method thereof

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