CN112494359B

CN112494359B - Preparation method of seaweed oligosaccharide and application of seaweed oligosaccharide in anti-aging cosmetics

Info

Publication number: CN112494359B
Application number: CN202011483838.2A
Authority: CN
Inventors: 盘学平
Original assignee: Guangzhou Shangzi Chemical Technology Co ltd
Current assignee: Guangzhou Shangzi Chemical Technology Co ltd
Priority date: 2020-12-15
Filing date: 2020-12-15
Publication date: 2021-08-31
Anticipated expiration: 2040-12-15
Also published as: CN112494359A

Abstract

The invention discloses a composition, comprising: seaweed oligosaccharide, volcanic mud, milk essence, edible glycerol, vitamin E and the like. The invention also discloses a preparation method of the composition, and the composition has the effects of moistening and moisturizing, reducing wrinkles and delaying senescence.

Description

Preparation method of seaweed oligosaccharide and application of seaweed oligosaccharide in anti-aging cosmetics

Technical Field

The invention belongs to the field of cosmetics, relates to a composition containing seaweed oligosaccharide and a preparation method and application thereof, and particularly relates to preparation of seaweed active oligosaccharide and application of seaweed active oligosaccharide in anti-aging cosmetics.

Background

The degree of modern environmental pollution, facial radiation from computers, mobile phones and the like for a long time, life pressure and the like aggravate the process of skin aging. At present, nutrients of skin are easily absorbed by seaweed mud and mineral mud facial masks on the market, so that the skin is dry and the aging degree is increased, the seaweed mud and mineral mud facial masks are not easy to clean after being used, and the effect is usually opposite. At present, a facial mask which can clean metabolic products of epidermal cells, eliminate excessive free radicals, provide active amino acids and various trace element components required by skin, recover young skin and the like, is easy to clean and does not cause residue is lacking in the market.

The use of seaweed as a medicine is recorded in the long history of China, Shennong herbal medicine book (the public yuan 452-536) of Nanqi ceramic hong Jing and describes the dietotherapy property and the utilization method. It also has effects of reducing blood lipid, resisting thrombi, relieving brain fatigue, promoting children development, improving immunity, and delaying aging.

The invention discloses an application of algal polysaccharide, belonging to the technical field of biomedicine and particularly relates to an application of algal polysaccharide, which is disclosed in Chinese patent CN 104814985A. Algal polysaccharides are used for preparing antiviral or immunological preparations. Cell models and in-vivo animal experiments show that the algal polysaccharide can obviously improve the immunity of animals, and can promote the generation of cell factors, the typing of T lymphocytes and the proliferation of mouse spleen cells, thereby activating the cellular immune response. The functional algal polysaccharide is natural polysaccharide extracted from kelp, gulfweed, ciliate desert-grass, eucheuma, ulva pertusa, enteromorpha, asparagus, Ascophyllum nodosum and other seaweeds, and can also be low molecular weight algal polysaccharide or algal oligosaccharide prepared by degrading algal polysaccharide through different preparation methods. The polysaccharide extract of a single seaweed or the polysaccharide extract mixture of a plurality of seaweeds can be used as a novel antiviral and immunopotentiator to be applied to livestock, fish, shrimp and shellfish feeds, and has wide application prospect.

Chinese patent CN107582422A discloses a titanium dioxide/algal polysaccharide composite nano-particle and a preparation method and application thereof. The method comprises the following steps: dissolving algal polysaccharide in water, adding a nano titanium dioxide ethanol suspension, uniformly mixing, adjusting the pH value of the system to 2-7, irradiating by using an ultraviolet lamp for reaction, separating slurry after the reaction is finished, and drying to obtain the titanium dioxide/algal polysaccharide composite nano particles. The invention has the advantages of low manufacturing cost, concentrated particle size distribution of nano particles, good particle dispersion performance and improved compatibility with oil phase, can obviously improve the ultraviolet resistance of products when being applied to cosmetics, particularly sunscreen products, can also react with high-activity free radicals generated by photochemical catalytic activity of nano titanium dioxide, eliminate the damage of the free radicals to skin, improve the defect of the nano titanium dioxide as a sunscreen agent and improve the product performance.

Chinese patent CN108746658A discloses a method for preparing algal polysaccharide nano-gold particles with antibacterial activity, which comprises the following steps: step 1, preparing a trehalose liquid with the concentration of 0.01-0.1 g/mL; step 2, preparing a chloroauric acid solution with the concentration of 0.1-10 mmol/L; step 3, uniformly mixing the trehalose solution prepared in the step 1 and the chloroauric acid solution prepared in the step 2 according to the volume ratio of 0.5: 1-2: 1, and reacting for a certain time to obtain nano gold sol; and 4, centrifuging the nano-gold sol prepared in the step 3, collecting the solid at the bottom of a centrifuge tube, removing the supernatant, sequentially washing the collected solid at the bottom for 2 times by using distilled water, ethanol and acetone respectively, ultrasonically dissolving the obtained solid by using distilled water, removing the residue at the bottom, centrifuging the supernatant, and drying to obtain the nano-gold solid powder. According to the preparation method of the algal polysaccharide nano-gold particles with antibacterial activity, algal polysaccharide and nano-gold particles are combined together, so that the antibacterial activity of pure nano-gold is improved.

However, the development and utilization of seaweed mainly comprise antioxidant substances such as seaweed polysaccharide, seaweed polyphenol, fucoxanthin and the like, and the utilization of seaweed oligosaccharide as an active ingredient of natural anti-aging cosmetics is still blank. The alga oligosaccharide has good nutrition and moisture-keeping effects due to the rich double bonds and active-OH, can promote the supply of skin nutrition and the excretion of metabolic waste, dilate peripheral blood vessels and improve the metabolism of skin cells, and has good health-care and maintenance effects on the skin. Therefore, the alginate oligosaccharide is prepared by optimizing the sodium alginate through a certain process, and is successfully applied to the anti-aging cosmetics, so that the preparation method has very important economic value and practical significance.

Disclosure of Invention

The invention aims to solve the problems in the prior art and provides an application of seaweed oligosaccharide and other components with excellent antioxidant activity as effective components in preparing anti-aging cosmetics.

The invention belongs to the field of marine biological resource utilization and cosmetics, and prepares a natural anti-aging mask with strong antioxidant and moisturizing effects by using seaweed oligosaccharide and volcanic rock mud as main raw materials and adding milk essence, edible glycerin, vitamin E and the like as auxiliary materials, so that the comprehensive utilization of resources is realized, and the natural anti-aging mask can be widely applied to the field of cosmetics. The production process is simple, efficient, green and environment-friendly, and is suitable for industrial production; the product has strong oxidation resistance, is green and natural, and the anti-aging mask prepared from the product can be used on the skin surfaces of hands, faces, necks and the like, and has the effects of moistening and preserving moisture, reducing wrinkles and delaying aging.

In a first aspect, the present invention provides a composition, the components of which comprise:

algal oligosaccharide, volcanic mud and auxiliary materials.

In some embodiments, the components of the composition comprise, by weight:

10-70 parts of algal oligosaccharide (such as 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, 60 parts and 65 parts), 15-60 parts of volcanic mud (20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts and 55 parts) and 3-50 parts of auxiliary materials (such as 5 parts, 10 parts, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts and 45 parts).

In some embodiments, the components of the composition comprise, by weight:

15-40 parts of algal oligosaccharide, 20-45 parts of volcanic mud and 5-40 parts of auxiliary materials.

In some embodiments, the components of the composition comprise, by weight:

15-40 parts of algal oligosaccharide, 20-45 parts of volcanic mud and 15-40 parts of auxiliary materials.

In some embodiments, the composition has a viscosity of 6000-10000 mPas (e.g., 6500 mPas, 7000 mPas, 7500 mPas, 8000 mPas, 8500 mPas, 9000 mPas, 9500 mPas).

In some embodiments, the algal oligosaccharides have a degree of polymerization of 3 to 15 (e.g., 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14).

In some embodiments, the algal oligosaccharide has a degree of polymerization of 4.2 to 9.7.

In some embodiments, the method of making algal oligosaccharides comprises the steps of:

s1: treating sodium alginate with alginate gel lyase to obtain crude cleavage product;

s2: centrifuging the crude cracking product, taking the supernatant and drying to obtain a fine cracking product;

s3: and crushing and screening the fine cracking product to obtain the algal oligosaccharide.

In some embodiments, in step S1, the concentration of sodium alginate in the reaction system is 0.3-2.0g/100mL (e.g., 0.5g/100mL, 0.8g/100mL, 1.0g/100mL, 1.2g/100mL, 1.4g/100mL, 1.6g/100mL, 1.8g/100mL) of aqueous solution, and the concentration of alginate lyase in the reaction system is 0.5-5 × 10⁴U/mL (e.g., 1X 10)⁴U/mL、1.5×10⁴U/mL、2.0×10⁴U/mL、2.5×10⁴U/mL、3.0×10⁴U/mL、3.5×10⁴U/mL、4.0×10⁴U/mL、4.5×10⁴U/mL)。

In some embodiments, in step S1, the temperature of the treatment is 25-40 deg.C (e.g., 28 deg.C, 30 deg.C, 32 deg.C, 34 deg.C, 36 deg.C, 38 deg.C).

In some embodiments, in step S1, the pH of the treatment is 6.0-9.0 (e.g., 6.5, 7.0, 7.5, 8.0, 8.5).

In some embodiments, in step S1, the processing time is 1-4h (e.g., 1.5h, 2.0h, 2.5h, 3.0h, 3.5 h).

In some embodiments, in step S2, the centrifugation is performed at 5000-.

In some embodiments, in step S2, the centrifugation time is 3-10 minutes (e.g., 4 minutes, 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes).

In some embodiments, in step S2, the drying is a film evaporation process.

In some embodiments, in step S3, the sieving is performed by sieving with a 100-200 mesh sieve and taking undersize.

In some embodiments, the specific surface area of the volcanic mud is 20-25m²G (e.g., 21 m)²/g、22m²/g、23m²/g、24m²/g)。

In some embodiments, the volcanic mud has a pore volume of 0.015 to 0.025cm³G (e.g., 0.016 cm)³/g、0.017cm³/g、0.018cm³/g、0.019cm³/g、0.020cm³/g、0.021m³/g、0.022cm³/g、0.023cm³/g、0.024cm³/g)。

In some embodiments, the volcanic mud has an average pore size of 3-4 nm.

In some embodiments, the volcanic mud has a particle size of 500-800 mesh.

In some embodiments, the preparation method of the volcanic mud comprises the following steps:

si: treating volcanic rock with acid to obtain coarse volcanic rock mud;

sii: drying the crude volcanic rock mud to obtain dried crude volcanic rock mud;

siii: and crushing and sieving the dried coarse volcanic mud, and taking undersize products to obtain the volcanic mud.

In some embodiments, in step Si, the acid is selected from one of hydrochloric acid, acetic acid, or lactic acid.

In some embodiments, in step Si, the acid is H⁺The concentration of (B) is 0.3-0.7 mol/L.

In some embodiments, in step Si, the volcanic rock is used in the acid in an amount of 20-40 g/L.

In some embodiments, in step Si, the temperature of the treatment is 50-85 deg.C (e.g., 55 deg.C, 60 deg.C, 65 deg.C, 70 deg.C, 75 deg.C, 80 deg.C).

In some embodiments, in step Si, the treatment time is 8-15h (e.g., 9h, 10h, 11h, 12h, 13h, 14 h).

In some embodiments, in step Si, the treatment is performed under stirring conditions.

In some embodiments, the crude volcanic mud is water washed to neutrality and then dried at step Sii.

In some embodiments, the drying is oven drying at 75-90 ℃ (e.g., 78 ℃, 80 ℃, 82 ℃, 84 ℃, 86 ℃, 88 ℃) at step Sii.

In some embodiments, in step Siii, the pulverizing is pulverizing with a nano-pulverizer.

In some embodiments, in step Siii, the sieving is through a 500-800 mesh sieve.

In some embodiments, the adjuvant comprises, by weight in the composition:

0-20 parts of nutrient substances (such as 2 parts, 4 parts, 6 parts, 8 parts, 10 parts, 12 parts, 14 parts, 16 parts and 18 parts), 5-15 parts of humectant (such as 6 parts, 8 parts, 10 parts, 12 parts and 14 parts), and 0-15 parts of vitamins (such as 2 parts, 4 parts, 6 parts, 8 parts, 10 parts, 12 parts and 14 parts).

In some embodiments, the adjuvant comprises, by weight in the composition:

5-20 parts of nutrient substances, 5-15 parts of humectant and 5-15 parts of vitamin.

In some embodiments, the nutrient is selected from milk serum.

In some embodiments, the humectant is selected from at least one of glycerin, hyaluronic acid, aloe vera, honey.

In some embodiments, the vitamin is selected from vitamin E.

In some embodiments, the adjuvant further comprises an amino acid.

In some embodiments, the amino acid is present in the composition in a weight ratio of 1 to 3 parts. In some embodiments, the amino acid can be any amino acid commonly used in the skin care product art, such as: repairing amino acids, moisturizing amino acids, healing promoting amino acids, antioxidant amino acids, and synergistic sunscreen amino acids. More specifically, the repair amino acids are selected from proline and/or arginine; the antioxidant amino acid can be glutathione and/or histidine; the healing promoting amino acid is arginine and/or glutamyl peptide; the synergistic sunscreen amino acid is histidine.

In a second aspect, the present invention provides a process for preparing a composition according to the first aspect of the present invention, said process comprising the steps of:

mixing the algal oligosaccharide, the volcanic mud and the auxiliary materials to obtain the composition.

In some embodiments, the method of making further comprises the steps of:

the viscosity of the composition was adjusted to 6000-10000 mPas with water.

In some embodiments, the method of making further comprises the steps of:

sterilizing the composition to obtain a sterilized composition.

In some embodiments, the sterilization is autoclaving.

In some embodiments, the temperature of the autoclaving is 110-.

In some embodiments, the pressure of the autoclaving is 0.8 to 0.15MPa (e.g., 1.0MPa, 1.2MPa, 1.4MPa).

In some embodiments, the autoclaving time is 5-15min (e.g., 6min, 8min, 10min, 12min, 14 min).

In a third aspect, the present invention provides the use of a composition according to the first aspect of the present invention or a method of manufacture according to the second aspect of the present invention in the manufacture of a formulation for anti-aging.

In some embodiments, the formulation is a skin care product or medicament. The skin care product may be a mask.

Drawings

FIG. 1 shows N in mineral composition of volcanic mud₂Adsorption-desorption curve.

Fig. 2 is a comparison chart of evaluation index results of the mask, in which the values of the wettability, the viscosity and the moisturizing effect of each composition tested are sequentially set from left to right among three columns of the composition tested.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below. The present invention is further illustrated by the following examples, but the scope of the present invention is not limited to the following examples.

Example 1

(1) Preparation of algal oligosaccharides:

taking sodium alginate water solution with mass concentration of 0.6g/100mL as a reaction system, adding the sodium alginate water solution into an enzymolysis tank, and simultaneously adding alginate gel lyase into the reaction system to ensure that the final concentration of the alginate gel lyase is 1 × 10²U/mL, adjusting the enzymolysis temperature to 25 ℃ and the pH value to 6.5, and carrying out enzymolysis for 3 h; and (3) treating the enzymatic hydrolysate after the enzymolysis is finished in a centrifugal machine, centrifuging at 5000rpm for 5min, concentrating the supernatant by using a membrane evaporation technology, drying to obtain seaweed oligosaccharide dry powder, crushing the seaweed oligosaccharide dry powder, sieving by using a 200-mesh sieve, and taking undersize products for later use to obtain the seaweed oligosaccharide. The polymerization degree of the obtained seaweed oligosaccharide is 5.4 by measurement.

Alginate gel lyase (1X 10)⁴U/mL): qingdao Baijie ocean biological resources, Inc.

(2) Preparing mineral components of volcanic mud:

selecting 30g of volcanic rock, putting the volcanic rock into a beaker filled with 1000mL0.5mol/L of acetic acid solution, putting the beaker into a water bath kettle at 80 ℃, stirring for 12h to form volcanic rock mud, washing the volcanic rock mud with deionized water until the volcanic rock mud is neutral, putting the prepared sample into an oven to be dried at 80 ℃, crushing the sample by a nano crusher, sieving the crushed sample with a 500-mesh sieve, and taking undersize materials for later use to obtain the volcanic rock mud.

The skin cleanser has a fluffy structure, has wide specific surface area and good porosity, is beneficial to adsorbing and removing redundant grease and dirt on the skin, and can play a better cleaning role; inhibiting sebum secretion, and removing old waste keratin.

N of the mineral component of the volcanic mud obtained by the invention₂The adsorption-desorption curve is shown in FIG. 1. Through testing, the specific surface area of the prepared volcanic mud is as follows: 23.6296m²(ii)/g; pore volume: 0.021104cm³(ii)/g; average pore diameter: 3.57253 nm. Other indexes of the prepared volcanic mud are shown in table 1.

TABLE 1 index of mineral composition of volcanic mud

(3) Uniformly mixing:

according to the weight parts, 20 parts of the algal oligosaccharide prepared in the step (1), 40 parts of the volcanic mud prepared in the step (2), 15 parts of milk essence, 10 parts of edible glycerin and 10 parts of vitamin E are added with distilled water to adjust the viscosity to 6000-10000mPa & s, so that the seaweed oligosaccharide is uniform and can be uniformly smeared on the skin.

(4) And (3) sterilization:

placing the product in an autoclave for sterilization treatment, wherein the temperature is as follows: 121 ℃, pressure: 0.12MPa, treatment time: and cooling for 10 minutes to obtain a finished product A1.

Example 2

(1) Preparation of algal oligosaccharides:

taking sodium alginate aqueous solution with mass concentration of 1.6g/100mL as a reaction system, adding the sodium alginate aqueous solution into an enzymolysis tank, and simultaneously adding alginate gel lyase into the reaction system to ensure that the final concentration of the alginate gel lyase is 1 × 10²U/mL, adjusting the enzymolysis temperature to 40 ℃ and the pH value to 8.0, and carrying out enzymolysis for 3 h; and (3) treating the algae liquid after the enzymolysis is finished in a centrifugal machine, centrifuging for 10min at 8000r, concentrating the supernatant by using a membrane evaporation technology, drying to obtain dry algal oligosaccharide powder, crushing the dry algal oligosaccharide powder, sieving by using a 200-mesh sieve, and taking undersize products for later use to obtain the algal oligosaccharide. The polymerization degree of the obtained seaweed oligosaccharide is 9.7 through measurement.

(2) Preparing mineral components of volcanic mud:

(3) Uniformly mixing:

according to the weight parts, 35 parts of the algal oligosaccharide prepared in the step (1), 30 parts of the volcanic mud prepared in the step (2), 15 parts of milk essence, 10 parts of edible glycerin and 10 parts of vitamin E are added with distilled water to adjust the viscosity to 6000-10000mPa & s, so that the seaweed oligosaccharide is uniform and can be uniformly smeared on the skin.

(4) And (3) sterilization:

placing the product in an autoclave for sterilization treatment, wherein the temperature is as follows: 121 ℃, pressure: 0.12MPa, treatment time: and cooling for 10 minutes to obtain a finished product A2.

Example 3

(1) Preparation of algal oligosaccharides:

taking sodium alginate aqueous solution with mass concentration of 0.8g/100mL as a reaction system, adding the sodium alginate aqueous solution into an enzymolysis tank, and simultaneously adding alginate gel lyase into the reaction system to ensure that the final concentration of the alginate gel lyase is 1 × 10²U/mL, adjusting the enzymolysis temperature to 25 ℃ and the pH value to 8.0, and carrying out enzymolysis for 3 h; and (3) treating the algae liquid after the enzymolysis is finished in a centrifugal machine, centrifuging for 8min at 5000r, concentrating the supernatant by using a membrane evaporation technology, drying to obtain dry algal oligosaccharide powder, crushing the dry algal oligosaccharide powder, sieving by using a 200-mesh sieve, and taking undersize products for later use to obtain the algal oligosaccharide. The polymerization degree of the obtained seaweed oligosaccharide is 4.2 by measurement.

(2) Preparing mineral components of volcanic mud:

(3) Uniformly mixing:

28 parts of algal oligosaccharide prepared in the step (1), 42 parts of volcanic mud prepared in the step (2), 10 parts of milk essence, 10 parts of edible glycerol and 10 parts of vitamin E by weight, and distilled water is added to adjust the viscosity to 6000-10000mPa & s, so that the seaweed oligosaccharide is uniform and can be uniformly smeared on skin.

(4) And (3) sterilization: placing the product in an autoclave for sterilization treatment, wherein the temperature is as follows: 121 ℃, pressure: 0.12MPa, treatment time: and cooling for 10 minutes to obtain a finished product A3.

Comparative example 1:

the difference from example 2 is that step (1) is omitted and in step (3) alginate is substituted for algal oligosaccharides.

The finished product C1 was obtained.

Comparative example 2:

the difference from example 2 is that step (2) is omitted, and in step (3), the volcanic mud mineral component is omitted.

The finished product C2 was obtained.

Comparative example 3:

the difference from example 2 is that in step (3), the milk essence is omitted.

The finished product C3 was obtained.

Comparative example 4:

the difference from example 2 is that in step (3), vitamin E is omitted.

The finished product C4 was obtained.

Test example: test of cosmetic products

The finished products A1, A2, A3, C1, C2, C3 and C4 were all applied masks and used in the tests described below.

(1) Sensory testing

70 skin aging patients are selected and are all female, and the age is 30 +/-3.5 years.

Inclusion criteria skin showed signs of aging: dry, fine lines, rough, yellow complexion, desquamation, irregular pigmentary changes or precipitated speckles; decreased skin elasticity, increased sensitivity, etc.

Exclusion criteria: the face has the conditions of damage, acne scar, erosion and the like, and patients with face allergy and patients using allergy-removing medicines or freckle-removing medicines.

After cleansing the face, they applied masks a1, a2, A3, C1, C2, C3, and C4 to the face, set each index to 1 to 5 points using the degree of moisturization, viscosity, and moisturizing effect as scoring criteria, and scored according to the applied feeling, 10 subjects per mask.

See table 2 for scoring criteria. The average value of the scoring result is shown in fig. 2, wherein three indexes corresponding to each facial mask are respectively and sequentially as follows: moisture, consistency, and moisturizing effect (i.e., moisture retention).

TABLE 2 mask score criteria points

Evaluation criteria	Poor effect	General effects	Good effect
				Moistening degree	1－2	3	4-5
Consistency of viscosity	1－2	3	4-5
				Moisture retention	1－2	3	4-5

(2) Radical scavenging experiments for compositions

Measurement of DPPH & free radical scavenging rate:

according to the method described in document 1 (research on enzymatic extraction process of chicken-derived collagen peptide and its radical scavenging ability), mussaenda gigantean et al, food industry, 2014, volume 35, phase 2, page 144-119), quantitative analysis was performed by spectroscopic method, 0.3g of each algal oligosaccharide composition (A1, A2, A3, C1, C2, C3, C4) was taken, placed in 50ml of anhydrous ethanol, stirred at room temperature for 12h, and 2ml of each sample solution and DPPH solution were taken as Ai (sample absorption inhibition value); the sample solution and absolute ethanol were Ac (sample control); DPPH solution and absolute ethanol are Aj (no absorption inhibition value); absolute ethanol is a control for uninhibited absorbance. The mixture was shaken well and mixed, and after standing at room temperature for 30min, the absorbance was measured at a wavelength of 517nm using a 1cm cuvette (two tubes were measured for each value at the same time).

DPPH.radical scavenging ratio was calculated according to the method described in the above-mentioned publication, and the results are shown in Table 4.

Hydroxyl radical scavenging rate:

according to the method described in reference 2 (spectrophotometry for removing hydroxy radical in traditional Chinese medicine), Chenguanhua et al, Spectroscopy and Spectroscopy, 2002,22(4), p. 636), samples A1, A2, A3, C1, C2, C3 and C4 were prepared into solutions (concentration: 6mg/mL) with a certain mass concentration, 1.0mL was added to a series of 10mL colorimetric tubes with a cover, and 1.4mL of crystal violet solution (2X 10)^-5mol·L^-1)、1.0mL Fe²⁺Solution (5X 10)^-3mol·L^-1)、0.4mL H₂O₂(1%) solution, 1.0mL Tris-HCl solution (pH 5.5), diluted to 10mL with redistilled water and shaken well, after standing for 5min, absorbance was measured at 588 nm. To add no H₂O₂The sample solution of (2) is used as a background tube. VC was used as a positive control.

The hydroxyl radical scavenging ratio was calculated according to the method described in the above-mentioned publication, and the results are shown in Table 4.

③ superoxide anion radical (ABTS)⁺) Clearance rate:

the superoxide anion radical scavenging rate was measured by the pyrogallol method according to the method described in the above-mentioned document 1. The corresponding absorbance was measured at 325nm, and VC was used as a positive control.

Calculated as described in the aforementioned literature, superoxide anion radical scavenging was obtained and the results are shown in Table 4.

TABLE 4 scavenging ability of each composition for free radical (% in units)

Serial number	Name (R)	DPPH	OH	ABTS	⁺
						1	A1	79	80	78
2	A2	98	99	98
					3	A3	92	93	91
4	C1	45	49	42
					5	C2	73	69	70
6	C3	89	90	91
					7	C4	91	89	90

Therefore, the composition prepared by the invention can effectively remove free radicals and has an antioxidant effect.

It will be appreciated by those skilled in the art that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The embodiments disclosed above are therefore to be considered in all respects as illustrative and not restrictive. All changes which come within the scope of or equivalence to the invention are intended to be embraced therein.

Claims

1. A composition, the components of the composition comprising:

10-70 parts of algal oligosaccharide, 15-60 parts of volcanic mud and 3-50 parts of auxiliary materials;

the polymerization degree of the seaweed oligosaccharide is 3-15;

the preparation method of the seaweed oligosaccharide comprises the following steps:

s3: crushing and screening the fine cracking product to obtain the algal oligosaccharide;

the specific surface area of the volcanic mud is 20-25 m/g;

the pore volume of the volcanic mud is 0.015-0.025cm high-speed plantation/g;

the average pore diameter of the volcanic mud is 3-4 nm;

the particle size of the volcanic mud is 500-800 meshes;

the preparation method of the volcanic mud comprises the following steps:

si: treating volcanic rock with acid to obtain coarse volcanic rock mud;

siii: crushing and sieving the dried coarse volcanic mud, and taking undersize products to obtain the volcanic mud;

in step Si, the acid is selected from one of hydrochloric acid, acetic acid or lactic acid;

the auxiliary materials comprise the following components in percentage by weight in the composition:

5-20 parts of milk essence, 5-15 parts of humectant and 5-15 parts of vitamin E;

the viscosity of the composition is 6000-10000 mPa.s.

2. The composition of claim 1, wherein the components of the composition comprise, by weight:

3. The composition of claim 2, wherein the components of the composition comprise, by weight:

4. The composition of claim 1, wherein the algal oligosaccharides have a degree of polymerization of 4.2 to 9.7.

5. The composition of claim 1, wherein in step S1, the concentration of sodium alginate in the reaction system is 0.3-2.0g/100mL aqueous solution, and the concentration of alginate lyase in the reaction system is 0.5-5X 10⁴U/mL。

6. The composition of claim 1, wherein in step S1, the temperature of the treatment is 25-40 ℃.

7. The composition of claim 1, wherein in step S1, the pH of the treatment is 6.0-9.0.

8. The composition of claim 1, wherein in step S1, the treatment time is 1-4 h.

9. The composition as claimed in claim 1, wherein in step S2, the rotation speed of the centrifugation is 5000-.

10. The composition of claim 1, wherein in step S2, the time of centrifugation is 3-10 minutes.

11. The composition of claim 1, wherein in step S2, the drying is a film evaporation process.

12. The composition of claim 1, wherein in step S3, the sieving is performed by sieving with a 100-200 mesh sieve and taking the undersize.

13. The composition of claim 1, wherein in step Si, H is in the acid⁺The concentration of (B) is 0.3-0.7 mol/L.

14. The composition of claim 1, wherein in step Si, the volcanic rock is present in the acid in an amount of 20-40 g/L.

15. The composition of claim 1, wherein in step Si, the temperature of the treatment is 50-85 ℃.

16. The composition of claim 1, wherein in step Si, the treatment time is 8 to 15 hours.

17. The composition of claim 1, wherein in step Si, the treatment is performed under agitation.

18. The composition of claim 1, wherein the crude volcanic mud is washed to neutrality and then subjected to the drying step Sii.

19. The composition of claim 1, wherein in step Sii, the drying is oven drying at 75-90 ℃.

20. The composition of claim 1, wherein in step Siii, the pulverizing is with a nano-pulverizer.

21. The composition of claim 1, wherein in step Siii, the sieving is through a 500-mesh and 800-mesh sieve.

22. The composition of claim 1, wherein the humectant is selected from at least one of glycerin, hyaluronic acid, aloe vera, and honey.

23. The composition of claim 1, wherein said excipient further comprises an amino acid.

24. The composition of claim 23, wherein said amino acid is present in said composition in a weight ratio of 1 to 3 parts.

25. The composition of claim 23, wherein the amino acid is selected from the group consisting of a repair amino acid, a moisturizing amino acid, a healing promoting amino acid, an antioxidant amino acid, a synergistic sunscreen amino acid; the repair amino acid is selected from proline and/or arginine; the antioxidant amino acid is histidine; the healing promoting amino acid is arginine; the synergistic sunscreen amino acid is histidine.

26. A process for preparing a composition according to any one of claims 1 to 25, comprising the steps of:

27. The method of claim 26, further comprising the steps of:

the viscosity of the composition was adjusted to 6000-10000 mPas with water.

28. The method of claim 26, further comprising the steps of:

sterilizing the composition to obtain a sterilized composition.

29. The method of claim 28, wherein the sterilization is autoclaving.

30. The method of claim 29, wherein the temperature of the autoclaving is 110-130 ℃.

31. The method of claim 29, wherein the autoclaving pressure is in the range of 0.8 to 0.15 MPa.

32. The method of claim 29, wherein the autoclaving is performed for a period of 5 to 15 minutes.

33. Use of a composition according to any one of claims 1 to 25 or a product of a method of manufacture according to claims 26 to 32 in the manufacture of a formulation for anti-aging.

34. The use according to claim 33, wherein the formulation is a skin care product or a medicament.