CN112076127A - Antioxidant, raw material preparation method thereof, humectant and raw material preparation method thereof - Google Patents

Antioxidant, raw material preparation method thereof, humectant and raw material preparation method thereof Download PDF

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CN112076127A
CN112076127A CN202011046467.1A CN202011046467A CN112076127A CN 112076127 A CN112076127 A CN 112076127A CN 202011046467 A CN202011046467 A CN 202011046467A CN 112076127 A CN112076127 A CN 112076127A
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raw material
humectant
mixing
citrus pectin
antioxidant
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CN112076127B (en
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聂艳峰
裴运林
岳凯婷
郭朝万
胡露
蒲艳
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Guangdong Marubi Biological Technology Co Ltd
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783—Angiosperms [Magnoliophyta]
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    • A61K8/00—Cosmetics or similar toiletry preparations
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    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
    • C08B37/0048—Processes of extraction from organic materials
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52—Stabilizers
    • A61K2800/522—Antioxidants; Radical scavengers

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Abstract

The application relates to the field of cosmetics, in particular to an antioxidant and a raw material preparation method thereof, a humectant and a raw material preparation method thereof. A method for preparing a humectant raw material comprises the following steps: mixing citrus pectin aqueous solution of 5-10mg/mL with H2O2Mixing the aqueous solutions, irradiating for 0.8-1.2h under ultraviolet light to obtain degradation product, and separating substances with molecular weight of 100kDa or more from the degradation product; wherein the citrus pectin is reacted with H2O2The mass ratio of (A) to (B) is 100: 2-5. The citrus pectin treated by the method has good moisture retention property, and can be used for preparing humectant, wherein the molecular weight of the obtained material is greater than or equal to 100 kDa. The method can also obtain substances with the molecular weight of 2kDa to 20kDa, and the substances have better capacity of scavenging free radicals and can be used for preparing antioxidants.

Description

Antioxidant, raw material preparation method thereof, humectant and raw material preparation method thereof
Technical Field
The application relates to the field of cosmetics, in particular to an antioxidant and a raw material preparation method thereof, a humectant and a raw material preparation method thereof.
Background
Citrus Pectin (Citrus Pectin, baiCP for short) exists in a long-chain carbohydrate structure, and has a molecular weight of 500-3000 kDa and an esterification degree of 20-75%. The natural citrus pectin is generally used as a food additive and has good gelling, stabilizing, emulsifying, thickening and suspending functions.
The inventors have discovered a new use of citrus pectin.
Disclosure of Invention
The embodiment of the application aims to provide an antioxidant and a raw material preparation method thereof, a humectant and a raw material preparation method thereof, and aims to provide a new application of citrus pectin.
In a first aspect, the present application provides a method for preparing a humectant raw material, comprising:
mixing citrus pectin aqueous solution of 5-10mg/mL with H2O2Mixing the aqueous solutions, irradiating for 0.8-1.2h under ultraviolet light to obtain degradation product, and separating substances with molecular weight of 100kDa or more from the degradation product;
wherein the citrus pectin is reacted with H2O2The mass ratio of (A) to (B) is 100: 1-5.
The citrus pectin treated by the method has good moisture retention property, and can be used for preparing humectant, wherein the molecular weight of the obtained material is greater than or equal to 100 kDa.
In some embodiments of the first aspect of the present application, the degradant is dialyzed against a 100kDa dialysis bag, and substances having a molecular weight greater than or equal to 100kDa are taken from the dialysis bag.
In some embodiments of the first aspect of the present application, the H2O2The volume fraction of the aqueous solution is 30-40%.
In some embodiments of the first aspect of the present application, the citrus pectin is prepared by:
mixing citrus peel with 0.3-0.5 vol% HCl, adjusting pH to 2.5-2.8, heating to 90-95 deg.C, maintaining the temperature for 1-2 hr, and filtering;
decolorizing the filtrate, adjusting pH to 3.5-4.5 with ammonia water, adding 92-97.5 vol% ethanol water solution to precipitate the system, and collecting the precipitate as citrus pectin;
optionally, the step of decolorizing the filtrate comprises: mixing the filtrate with activated carbon, keeping the temperature at 80-84 deg.C for 30-40min, and filtering.
In a second aspect of the present application, a humectant is provided, and the raw material of the humectant comprises a product prepared by the preparation method of the humectant raw material provided in the first aspect.
The humectant provided by the embodiment of the application has excellent water locking performance, and the moisturizing effect of the humectant is superior to that of hyaluronic acid.
In a third aspect, the present application provides a method for preparing an antioxidant raw material, which mainly comprises:
mixing citrus pectin aqueous solution of 5-10mg/mL with H2O2Mixing the aqueous solutions, irradiating for 3-3.5h under ultraviolet light to obtain degradation products, and separating substances with molecular weight of more than or equal to 2kDa and less than 20kDa from the degradation products;
wherein the citrus pectin is reacted with H2O2The mass ratio of (A) to (B) is 100: 9-15.
After the citrus pectin is treated by the method, a substance with the molecular weight of 2kDa to 20kDa can be obtained, and the substance has better capacity of eliminating free radicals and can be used for preparing antioxidants.
In some embodiments of the third aspect of the present application, the degradant is dialyzed against a 2kDa dialysis bag, and substances having a molecular weight greater than or equal to 2kDa are removed from the dialysis bag.
In some embodiments of the third aspect of the present application, the H2O2Aqueous solutionThe volume fraction of (A) is 30-40%.
In some embodiments of the third aspect of the present application, the citrus pectin is prepared by:
mixing citrus peel with 0.3-0.5 vol% HCl, adjusting pH to 2.5-2.8, heating to 90-95 deg.C, maintaining the temperature for 1-2 hr, and filtering;
decolorizing the filtrate, adjusting pH to 3.5-4.5 with ammonia water, adding 92-97.5 vol% ethanol water solution to precipitate the system, and collecting the precipitate as citrus pectin;
optionally, the step of decolorizing the filtrate comprises: mixing the filtrate with activated carbon, and keeping the temperature at 80-84 deg.C for 30-40 min.
In a fourth aspect, the present application provides an antioxidant, and the raw material of the antioxidant includes a product obtained by the method for producing the raw material of the antioxidant provided in the third aspect.
The antioxidant provided by the embodiment of the application has better antioxidant capacity.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following specifically describes the antioxidant and the method for preparing the raw material thereof, the humectant and the method for preparing the raw material thereof in the examples of the present application.
A method for preparing a humectant raw material comprises the following steps:
mixing citrus pectin aqueous solution of 5-10mg/mL with H2O2Mixing the aqueous solutions, irradiating for 0.8-1.2h under ultraviolet light to obtain degradation product, and separating substances with molecular weight of 100kDa or more from the degradation product;
wherein the citrus pectin is reacted with H2O2The mass ratio of (A) to (B) is 100: 1-5.
In the examples of the present application, citrus pectin is made using the following method:
mixing citrus peel with 0.3-0.5 vol% HCl, adjusting pH to 2.5-2.8, heating to 90-95 deg.C, maintaining the temperature for 1-2 hr, and filtering;
decolorizing the filtrate, adjusting pH to 3.5-4.5 with ammonia water, adding 92-97.5 vol% ethanol water solution to precipitate the system, and collecting the precipitate as citrus pectin.
For example, dried citrus peel is mixed with 0.3-0.5 vol% (e.g., 0.3 vol%, 0.4 vol%, or 0.5 vol%) aqueous HCl, adjusted to pH 2.5-2.8, heated to 90-95 deg.C (e.g., 90 deg.C, 91 deg.C, 93 deg.C, or 95 deg.C, etc.), incubated for 1-2h (e.g., 1h, 1.2h, 1.4h, 1.6h, 1.8h, or 2h, etc.), and filtered.
Filtering, decolorizing the filtrate, in the examples of the present application, mixing the filtrate with activated carbon, and keeping the temperature at 80-84 deg.C (such as 80 deg.C, 81 deg.C, 82 deg.C, 83 deg.C, or 84 deg.C, etc.) for 30-40min (such as 30min, 32min, 35min, 38min, 39min, or 40min, etc.). Adsorbing the colored substances in the filtrate by using activated carbon, and separating to obtain the filtrate.
In other embodiments of the present application, other substances such as molecular sieves and the like may be mixed with the filtrate and then separated to achieve the purpose of decoloring the filtrate.
Decolorizing the filtrate, adjusting pH to 3.5-4.5 with ammonia water, adding 92-97.5 vol% ethanol water solution to precipitate the system, and collecting the precipitate as citrus pectin.
Illustratively, the volume fraction of the aqueous ethanol solution may be 92 vol%, 93 vol%, 95 vol%, 97 vol%, or 97.5 vol%, and so on.
In some embodiments, the citrus pectin may also be dried to a powder.
In this example, citrus pectin was prepared using the method described above. It should be noted that in other embodiments of the present application, citrus pectin can be prepared by other methods, or obtained by commercially available methods.
Preparing citrus pectin, and mixing with the citrus glue solution H2O2Mixing the aqueous solutions, and then subjecting the mixture to ultraviolet lightIrradiating for degradation, and separating to obtain substances with molecular weight of 100kDa or more to obtain humectant raw material.
The concentration of the aqueous citrus pectin solution is 5-10mg/mL, and may be, for example, 5mg/mL, 6mg/mL, 7mg/mL, 8mg/mL, 9mg/mL, 10mg/mL, or the like.
H2O2The concentration of the aqueous solution is 30-40% by volume, and may be, for example, 30%, 31%, 35%, 37%, 39%, or 40%, and so on.
Citrus pectin and H2O2The mass ratio of (A) to (B) is 100: 2-5. In other words, the citrus pectin and H in the aqueous citrus pectin solution2O2H in aqueous solution2O2The mass ratio of (A) to (B) is 100:2. 100:2.8, 100:3, 100:3.5, 100:4, or 100: 5, etc.
In other embodiments of the present application, H is2O2The volume concentration of the aqueous solution may also be other values.
The time of ultraviolet irradiation is 0.8-1.2h, for example, 0.8h, 0.9h, 1.1h or 1.2 h.
Orange glue solution in H2O2And decomposing under ultraviolet irradiation to obtain degradation product, and separating out substances with molecular weight of 100kDa or more.
In other embodiments of the present application, the degradant is dialyzed using a 100kDa dialysis bag, and substances with a molecular weight greater than or equal to 100kDa are taken from the bag.
In other embodiments of the present application, other means may be used to isolate substances having a molecular weight greater than or equal to 100kDa as humectant material.
The preparation method of the humectant raw material provided by the embodiment of the application is simple, the raw materials adopted in the preparation process are easy to obtain, and the product obtained by the preparation method of the humectant raw material has excellent moisturizing performance.
The application also provides a humectant, and the raw materials of the humectant comprise a product prepared by the preparation method of the humectant raw material. The humectant raw material has better moisturizing performance and better water locking performance.
The application also provides a preparation method of the antioxidant raw material, which mainly comprises the following steps:
mixing citrus pectin aqueous solution of 5-10mg/mL with H2O2Mixing the aqueous solutions, and irradiating for 3-3.5h under ultraviolet light to obtain degradation product, wherein substances with molecular weight of 2kDa or more and less than 20kDa are separated out from the degradation product.
Wherein the citrus pectin is reacted with H2O2The mass ratio of (A) to (B) is 100: 9-15.
In view of the above, in the examples of the present application, the method for preparing citrus pectin can be the method described above; or, the method is directly commercially available, and the like, and will not be described herein.
Mixing the citrus pectin aqueous solution with H2O2Mixing the aqueous solution, citrus pectin and H2O2The mass ratio of (A) to (B) is 100: 9-15. Irradiating for 3-3.5h under ultraviolet light to obtain degradation product, and separating substances with molecular weight of 2kDa or more and less than 20kDa to obtain antioxidant raw material.
In the present application, the concentration of the aqueous citrus pectin solution is 5-10mg/mL, and may be, for example, 5mg/mL, 5.1mg/mL, 6.2mg/mL, 7.4mg/mL, 8.1mg/mL, 8.9mg/mL, 10mg/mL, and the like.
H2O2The concentration of the aqueous solution is 30-40% by volume, and may be, for example, 30%, 31%, 35%, 36.5%, 37%, 39%, 40%, or the like.
Citrus pectin and H2O2The mass ratio of (A) to (B) is 100: 9-15. In other words, the citrus pectin and H in the aqueous citrus pectin solution2O2H in aqueous solution2O2The mass ratio of (A) to (B) is 100:9. 100:9.7, 100:10.2, 100:11, 100:12, 100: 13 or 100: 15, etc.
In other embodiments of the present application, H is2O2The volume concentration of the aqueous solution may also be other values.
The time of ultraviolet irradiation is 3-3.5h, for example, 3h, 3.1h, 3.2h, 3.4h or 3.5h, etc.
After the degradation product is obtained by decomposition, dialyzing the degradation product by using a 2kDa dialysis bag, and taking a substance with the molecular weight being more than or equal to 2kDa in the dialysis bag.
The antioxidant is prepared by adopting a citrus pectin decomposition mode, the method takes citrus pectin as a raw material, the raw material and reagents used in the preparation process are easy to obtain, and the preparation conditions are simple and not harsh; the obtained antioxidant has good free radical scavenging ability.
The application also provides an antioxidant, and the raw material of the antioxidant comprises a product prepared by the preparation method of the antioxidant raw material.
The product prepared by the preparation method of the antioxidant raw material has better antioxidant capacity, and the DPPH clearance of the antioxidant raw material can reach 90.2%.
The features and properties of the present application are described in further detail below with reference to examples.
Example 1
The embodiment provides a humectant raw material, which is mainly prepared by the following method:
adding 0.3 vol% HCl solution into dried citrus peel, immersing the peel, adjusting pH to 2.5, heating to 90 deg.C, maintaining the temperature for 1h, adding water and HCl solution during the temperature maintaining process to maintain pH at 2.5, and filtering while hot to obtain filtrate.
Adding 2% active carbon into the filtrate, and heating at 80 deg.C for 30min for decolorizing; decolorizing, filtering, cooling the filtrate, adjusting pH to 4 with dilute ammonia water, adding 95 vol% ethanol with three times volume to completely precipitate pectin, and vacuum drying the pectin precipitate to obtain powder.
Dissolving Mandarin orange pectin powder in water to obtain 10mg/mL pectin aqueous solution, adding 10 μ L H into 10mL pectin aqueous solution2O2H with the volume fraction of the aqueous solution of 36.5 percent2O2Uniformly mixing the aqueous solution, and then performing exposition under ultraviolet light for 1h to obtain a degradation product. Concentrating the degradation product to 5mL under vacuum at 60 ℃; dialyzing the degraded material with 100kDa dialysis bag, collecting substances with molecular weight of 100kDa or more in the dialysis bag, concentrating, and drying to obtain moisture-keeping substancePreparing raw materials.
The embodiment also provides a humectant which comprises the humectant raw material and an auxiliary material.
Example 2
This example provides a raw antioxidant material made essentially by the following process:
this example used the procedure of example 1 to produce citrus pectin powder.
Dissolving Mandarin orange pectin powder in water to obtain pectin aqueous solution with concentration of 10mg/mL, adding pectin aqueous solution 10mL, and adding 30 μ L H2O2H with the volume fraction of the aqueous solution of 36.5 percent2O2Uniformly mixing the aqueous solution, and then performing exposition under ultraviolet light for 3h to obtain a degradation product. Vacuum concentrating at 60 deg.C to 5 mL; dialyzing the degradation product by using a 2kDa dialysis bag, taking a substance with the molecular weight being more than or equal to 2kDa in the dialysis bag, concentrating and drying to obtain the antioxidant raw material.
Test example 1
The humectant raw material obtained in example 1 was mixed with water, carbomer, isopropyl alcohol and glycerin to prepare an aqueous phase, and isopropyl myristate, methyl dextran sesquistearate, ethylhexyl palmitate and mixed alcohol to prepare an oil phase. Mixing the water phase and the oil phase to obtain the humectant.
Wherein, five groups of humectants are prepared, each humectant is only different in the content of the humectant raw material prepared in example 1 in the humectant, and the mass fractions of the humectant raw materials prepared in example 1 in the five groups of humectants are respectively 0%, 0.04%, 0.08%, 0.12% and 0.16%.
Skin moisture test (MMV test): 30 volunteers aged 16-65 years are selected, have no severe allergic history, and are marked with 3cm by 3cm test areas on the inner sides of the left and right arms, and the same arm can be marked with multiple areas at intervals of 1 cm. Five groups of moisturizers were randomly distributed on the left and right arms and tested using a capacitance skin tester for the test area and the control area, each area being tested 5 times in parallel. When the skin care product is applied, the skin care product is applied according to the concentration, and after the skin care product is applied, the moisture content of the skin is respectively tested at 1 hour, 2 hours and 4 hours after the skin care product is applied.
Skin moisture loss test (TEWL method): the moisture content emitted by epidermis can be directly measured by the water vapor pressure gradient formed by the water loss of the cuticle at two different points by measuring the near epidermis (within 1 cm) through 2 groups of temperature and humidity sensors. The TEWL value is an important indicator of the quality of the skin barrier, and a lower TEWL value indicates a better barrier function of the skin, whereas a worse TEWL value indicates a poorer barrier function of the skin. The test results are shown in table 1.
TABLE 1 TEWL experimental results
Figure BDA0002706707760000091
The results of the MMV experiments show that the moisture retention of the emulsion added with 0.16% of the macromolecular citrus pectin is the best, and the skin moisture loss rate of the volunteers is reduced the most. The water loss rate was not significantly changed in the emulsion application zone where no macromolecular citrus pectin was added.
The results of the TEWL experiments show that the water dispersion of the test zone coated with the emulsion containing the humectant material prepared in example 1 gradually decreased and decreased with increasing addition. While the water dispersibility of the blank and the area coated with the humectant raw material prepared in example 1 was not significantly changed.
Test example 2
The humectant raw material obtained in example 1 was mixed with water, carbomer, isopropyl alcohol and glycerin to prepare an aqueous phase, and isopropyl myristate, methyl dextran sesquistearate, ethylhexyl palmitate and mixed alcohol to prepare an oil phase. The first humectant is prepared by mixing the water phase and the oil phase. In the humectant, the content of the humectant raw material prepared in example 1 was 0.16%.
The antioxidant material prepared in example 2 was mixed with water, carbomer, isopropanol and glycerin to prepare an aqueous phase, isopropyl myristate, methyl dextran sesquistearate, ethylhexyl palmitate and mixed alcohols to prepare an oil phase. And mixing the water phase and the oil phase to obtain a second humectant. In the humectant, the content of the humectant raw material prepared in example 1 was 0.16%.
The first moisturizing agent and the second moisturizing agent were used in 30 volunteers and tested by the epidermal water loss test (TEWL method) shown in test example 1, and the test results were averaged and shown in table 2.
TABLE 2 TEWL experimental results distribution for different moisturizers
Figure BDA0002706707760000101
Figure BDA0002706707760000111
It can be seen from Table 2 that the first moisturizing agent has a good moisturizing property and the second moisturizing agent has almost no moisturizing property.
Description of the drawings: the raw materials of the moisturizing agent provided in the embodiment 1 of the present application have a good moisturizing effect. The raw material of the antioxidant provided in example 2 of the present application has almost no moisturizing effect.
Test example 3
OH is a relatively active free radical and has strong attack capability. By means of fenton reaction to produce hydroxyl radical, H2O2+Fe2+＝·OH+H2O+Fe3+Salicylic acid is added into a reaction system, hydroxyl radicals generated by Fenton reaction react with the salicylic acid to generate 2, 3-dihydroxybenzoic acid with special absorption at 510nm, and if an object to be detected with the function of removing the hydroxyl radicals is added into the reaction system, the content of the free radicals is reduced, so that the generation amount of colored compounds is correspondingly reduced, the absorbance is reduced, and the free removal capacity can be evaluated.
1mL of the antioxidant raw material prepared in example 2 and having a mass concentration of 10mg/mL, and 2mL of 0.02 wt% FeSO were added to a dry tube4The solution, 1.5mL of a 1.8mmol/L salicylic acid-ethanol solution, and finally 0.1mL of 0.03% H2O2Shaking, and keeping at 37 deg.CHeating for 30 min; the first control group used distilled water instead of the antioxidant raw material prepared in example 2. The second control group used the humectant raw material prepared in example 1 in place of the antioxidant raw material prepared in example 2.
The absorbance at 510nm was measured and the clearance of free radicals by pectin was calculated according to the following formula:
OH clearance (%) ═ aSample (I)-AControl)/AControl*100％
The test results show that the humectant raw material prepared in example 1 has no obvious free radical scavenging effect; the raw antioxidant prepared in example 2 has a hydroxyl radical scavenging rate of 92.4%.
Test example 4
DPPH, also known as 1, 1-diphenyl-2-trinitrophenylhydrazine, is a very stable free radical with a nitrogen center, and the stability of DPPH is mainly caused by steric hindrance of 3 benzene rings with resonance stabilization, so that unpaired electrons on the nitrogen atom in the middle cannot play the role of electron pairing. Its absolute ethyl alcohol solution is purple, and has maximum absorption at wavelength of 517nm, and its absorbance and concentration are in linear relation. When a radical scavenger is added thereto, DPPH may be combined with or substituted for the radical scavenger, whereby the radical scavenging ability can be evaluated by decreasing the number of radicals, decreasing the absorbance, and decreasing the color of the solution.
Preparing 0.2mmol/L DPPH-methanol (or absolute ethyl alcohol) solution; preparing a humectant raw material aqueous solution with the concentration of 10mg/mL, which is prepared in the example 1; an aqueous solution of the antioxidant material prepared in example 2 was prepared at a concentration of 10 mg/mL. VC solution with the concentration of 10mg/mL is prepared.
Three test tubes, 2mL of the humectant raw material aqueous solution prepared in example 1, 2mL of the antioxidant raw material aqueous solution prepared in example 2, and 2mL of the VC solution were each aspirated.
Respectively adding 2ml of PPH solution into the test tubes, mixing, reacting in dark for 30min, and measuring the light absorption value A at 517nm1。
Separately, 2mL of the aqueous humectant material solution prepared in example 1 and 2mL of the aqueous humectant material solution prepared in example 2 were taken out of the three test tubesThe obtained antioxidant raw material aqueous solution and 2mL of VC solution. Adding 2mL of methanol into the test tube, mixing, reacting in dark for 30min, and measuring the light absorption A at 517nm2。
Sucking 2mL of the solution and 2mL of methanol into a test tube with a plug, mixing uniformly, reacting for 30min in a dark place, and measuring the light absorption value A at the wavelength of 517nm0(ii) a 3 replicates were made for each sample.
DPPH clearance was calculated according to the following formula:
Figure BDA0002706707760000131
the test results show that the humectant raw material prepared in example 1 has no obvious free radical scavenging effect; the raw antioxidant prepared in example 2 has a hydroxyl radical scavenging rate of 90.2%.
In conclusion, the humectant raw material prepared in the embodiment 1 of the application has better moisturizing performance; the water locking effect is better. The antioxidant material prepared in example 2 had almost no moisturizing properties, although the preparation method was much similar to that of example 1. The antioxidant raw material prepared in example 2 has a good radical scavenging effect and a good antioxidant capacity, and the humectant raw material prepared in example 1 has almost no radical scavenging capacity.
The humectant raw material prepared in example 1 was suitable for preparing a humectant, and the antioxidant raw material prepared in example 2 was suitable for preparing an antioxidant.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims (10)

1. A preparation method of a humectant raw material is characterized by comprising the following steps:
mixing citrus pectin aqueous solution of 5-10mg/mL with H2O2Mixing the aqueous solutions, irradiating for 0.8-1.2h under ultraviolet light to obtain degradation product, and separating substances with molecular weight of 100kDa or more from the degradation product;
wherein the citrus pectin is reacted with H2O2The mass ratio of (A) to (B) is 100: 1-5.
2. The method for preparing the humectant raw material according to claim 1, wherein the degradation product is dialyzed using a 100kDa dialysis bag, and a substance having a molecular weight of 100kDa or more in the dialysis bag is taken.
3. The method for preparing the humectant raw material according to claim 1, wherein the H is2O2The volume fraction of the aqueous solution is 30-40%.
4. The method for producing a humectant raw material according to claim 1, characterized in that,
the citrus pectin is prepared by the following steps:
mixing citrus peel with 0.3-0.5 vol% HCl, adjusting pH to 2.5-2.8, heating to 90-95 deg.C, maintaining the temperature for 1-2 hr, and filtering;
decolorizing the filtrate, adjusting pH to 3.5-4.5 with ammonia water, adding 92-97.5 vol% ethanol water solution to precipitate the system, and collecting the precipitate as citrus pectin;
optionally, the step of decolorizing the filtrate comprises: mixing the filtrate with activated carbon, keeping the temperature at 80-84 deg.C for 30-40min, and filtering.
5. A humectant characterized in that a raw material of the humectant comprises a product obtained by the production method of the humectant raw material according to any one of claims 1 to 4.
6. The preparation method of the antioxidant raw material is characterized by mainly comprising the following steps:
mixing citrus pectin aqueous solution of 5-10mg/mL with H2O2Mixing the aqueous solutions, irradiating for 3-3.5h under ultraviolet light to obtain degradation products, and separating substances with molecular weight of more than or equal to 2kDa and less than 20kDa from the degradation products;
wherein the citrus pectin is reacted with H2O2The mass ratio of (A) to (B) is 100: 9-15.
7. The method for preparing raw material for antioxidants according to claim 6, characterized in that the degradation product is dialyzed using a dialysis bag of 2kDa, and substances having a molecular weight of 2kDa or more in the dialysis bag are taken.
8. The method of claim 6, wherein the H is selected from the group consisting of2O2The volume fraction of the aqueous solution is 30-40%.
9. The method for producing an antioxidant raw material as set forth in any one of claims 6 to 8,
the citrus pectin is prepared by the following steps:
mixing citrus peel with 0.3-0.5 vol% HCl, adjusting pH to 2.5-2.8, heating to 90-95 deg.C, maintaining the temperature for 1-2 hr, and filtering;
decolorizing the filtrate, adjusting pH to 3.5-4.5 with ammonia water, adding 92-97.5 vol% ethanol water solution to precipitate the system, and collecting the precipitate as citrus pectin;
optionally, the step of decolorizing the filtrate comprises: mixing the filtrate with activated carbon, and keeping the temperature at 80-84 deg.C for 30-40 min.
10. An antioxidant, wherein the raw material of the antioxidant comprises a product obtained by the method for producing the raw material of the antioxidant according to any one of claims 6 to 9.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023006108A1 (en) * 2021-07-30 2023-02-02 梅晔生物医药股份有限公司 Sodium hyaluronate having full molecular weight distribution, preparation method therefor, and use thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2441024C1 (en) * 2010-07-21 2012-01-27 Учреждение Российской академии наук Институт биологии моря им. А.В. Жирмунского Дальневосточного отделения РАН Method of producing low-molecular pectin
ES2537936A1 (en) * 2013-12-11 2015-06-15 Universidad Miguel Hernández De Elche Production method of modified citrus pectin (Machine-translation by Google Translate, not legally binding)
CN106361633A (en) * 2016-09-06 2017-02-01 中国科学院重庆绿色智能技术研究院 Moisturizing mask prepared from citrus peel pomace and preparation method thereof
CN107141369A (en) * 2017-05-25 2017-09-08 华南理工大学 A kind of preparation method of modified pectin

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2441024C1 (en) * 2010-07-21 2012-01-27 Учреждение Российской академии наук Институт биологии моря им. А.В. Жирмунского Дальневосточного отделения РАН Method of producing low-molecular pectin
ES2537936A1 (en) * 2013-12-11 2015-06-15 Universidad Miguel Hernández De Elche Production method of modified citrus pectin (Machine-translation by Google Translate, not legally binding)
CN106361633A (en) * 2016-09-06 2017-02-01 中国科学院重庆绿色智能技术研究院 Moisturizing mask prepared from citrus peel pomace and preparation method thereof
CN107141369A (en) * 2017-05-25 2017-09-08 华南理工大学 A kind of preparation method of modified pectin

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
岳凯婷: "基于光催化过氧化氢氧化反应的改性柑橘果胶制备及其结构与性能研究", 《中国优秀硕士学位论文全文数据库》 *
李英华等: "高分子果胶与改性果胶的吸湿保湿性能比较研究", 《天然产物研究与开发》 *
阳晖: "《食品工艺学实验》", 31 May 2019, 西南交通大学出版社 *
陈剑兵等: "亚临界水改性果胶的抗氧化和抗肿瘤活性研究", 《食品科技》 *
马丽苹等: "改性苹果果胶性质及抗氧化活性", 《食品科学》 *
魏子淏等: "改性柑橘果胶研究进展", 《中国食品添加剂》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023006108A1 (en) * 2021-07-30 2023-02-02 梅晔生物医药股份有限公司 Sodium hyaluronate having full molecular weight distribution, preparation method therefor, and use thereof
US11976139B2 (en) 2021-07-30 2024-05-07 Meyer Bio-medicine Co., Ltd. Sodium hyaluronate with full molecular weight distribution (MWD), and preparation method and use thereof

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