CN108354864B - Preparation method of emulsion with whitening and moisturizing effects - Google Patents
Preparation method of emulsion with whitening and moisturizing effects Download PDFInfo
- Publication number
- CN108354864B CN108354864B CN201810293810.9A CN201810293810A CN108354864B CN 108354864 B CN108354864 B CN 108354864B CN 201810293810 A CN201810293810 A CN 201810293810A CN 108354864 B CN108354864 B CN 108354864B
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- emulsion
- whitening
- liquid
- oil phase
- weighing
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Classifications
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- A61K2800/782—Enzyme inhibitors; Enzyme antagonists
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Abstract
The invention provides a preparation method of an emulsion with whitening and moisturizing effects, which comprises the following steps: (1) weighing hydrogenated soybean oil, and heating to 75-85 ℃ to obtain a liquid oil phase I; (2) weighing arbutin, ascorbyl glucoside and nicotinamide in proportion, and mixing the three substances to obtain a composite whitening active substance; (3) adding the composite whitening active substance into the liquid oil phase I according to a certain proportion, and uniformly mixing to obtain a liquid oil phase II; (4) weighing the algal polysaccharide enzymolysis product, phospholipid and distilled water according to a proportion, heating to 75-85 ℃, and uniformly mixing to obtain a liquid water phase; (5) weighing the liquid oil phase II, the liquid water phase and the tea polyphenol according to the proportion, mixing and stirring uniformly to obtain a mixed solution, and homogenizing the mixed solution at high pressure to obtain the nano emulsion; and cooling the obtained nano emulsion to room temperature, and adding a proper amount of preservative to obtain the emulsion with the whitening and moisturizing effects. The emulsion prepared by the invention has whitening and moisturizing effects and good stability.
Description
(I) technical field
The invention belongs to the technical field of cosmetics, and particularly relates to a preparation method of an emulsion with whitening and moisturizing effects.
(II) technical background
The whitening is always paid great attention by people, and whitening skin care products are continuously advocated and pursued by women. The difference in skin color of a human body generally depends on factors such as the content and distribution of melanin in the epidermis, the collagen fiber structure of the dermis, and the thickness and water content of the stratum corneum.
At present, most whitening skin care products on the market generally have the problem of single whitening mechanism: the product only aims at the formation and transfer mechanism of melanin, carries out whitening formula design from three steps of inhibiting tyrosinase activity, reducing the produced melanin and inhibiting the transfer of the melanin, and cannot realize full-effect whitening. And the product stability is poor, and because the whitening agent is easily oxidized and inactivated or decomposed under illumination, if the whitening agent is directly added into a formula, the product is easily discolored and smells, and even the problems of paste layering, thickening and the like are caused.
Patent CN 107374988A discloses a preparation method of nonionic vesicles with whitening effect. The processing method comprises the steps of taking a traditional whitening agent, hydroxyphenoxypropionic acid, phloretin, hydroxytyrosol, a comfrey root extract and polyhydric alcohol as whitening components, taking glyceryl oleate citrate, cetearyl glucoside and polyglycerol-3-methyl glucose distearate as nonionic surfactant premix, and homogenizing to obtain the nonionic vesicle with the whitening effect. However, the method uses a nonionic surfactant, and cannot effectively wrap all active ingredients.
Patent CN 103690380 a discloses a method for preparing a whitening nanoparticle emulsion with a solid phase core, in the method, paeonol, a daisy flower extract, ribes nigrum seed oil and mandelic acid are used as whitening agents, glyceryl stearate, cetearyl ether-20 and cetearyl ether-12 are used as emulsifiers, and the whitening nanoparticle emulsion with the solid phase core is obtained through homogenization and cooling. The emulsion prepared by the method has a granular feeling due to the solid core, and gives a feeling that the active ingredient is not completely dissolved.
Disclosure of the invention
The invention aims to provide a preparation method of an emulsion with whitening and moisturizing effects and good stability.
The technical scheme of the invention is specifically explained as follows:
the invention provides a preparation method of an emulsion with whitening and moisturizing effects, which comprises the following steps:
(1) weighing hydrogenated soybean oil, and heating to 75-85 ℃ to obtain a liquid oil phase I;
(2) weighing arbutin, ascorbyl glucoside and nicotinamide according to the mass ratio of 2-4: 3-6: 1, and mixing the three substances to obtain a composite whitening active substance;
(3) adding the composite whitening active substance into the liquid oil phase I obtained in the step (1), and uniformly mixing to obtain a liquid oil phase II; wherein the mass ratio of the composite whitening active substance to the liquid oil phase I is 0.15-0.30: 1;
(4) according to the mass ratio of 0.08-0.2: weighing the algal polysaccharide enzymolysis product, phospholipid and distilled water according to the ratio of 0.05-0.1: 1, heating to 75-85 ℃, and uniformly mixing to obtain a liquid water phase;
(5) according to the mass ratio of 15-25: 120-150: 1, weighing the liquid oil phase II obtained in the step (3), the liquid water phase obtained in the step (4) and tea polyphenol, mixing and stirring uniformly to obtain a mixed solution, carrying out high-pressure homogenization on the mixed solution in a high-pressure homogenizer to obtain nano emulsion, and ensuring that the temperature of the mixed solution at an outlet section of the high-pressure homogenizer is not more than 90 ℃; and cooling the obtained nano emulsion to room temperature, and adding a proper amount of preservative to obtain the emulsion with the whitening and moisturizing effects.
In the invention, the seaweed polysaccharide enzymolysis product is prepared by the following method: extracting seaweed with water, precipitating with ethanol to obtain seaweed polysaccharide, and performing enzymolysis on the seaweed polysaccharide with dextranase to obtain seaweed polysaccharide enzymolysis product. The specific operation steps are as follows:
(a) the extraction method of algal polysaccharide comprises the steps of cleaning seaweed, drying and crushing to obtain algal powder, soaking and degreasing the algal powder in 95% ethanol solution by volume, standing overnight, adding distilled water into the degreased algal powder according to the material-liquid ratio of 1kg: 8-12L (preferably 1kg: 10L), carrying out water bath for 1-3 hours (preferably 2 hours) at 80-100 ℃ (preferably 95 ℃), cooling and standing for 0.5-1.5 hours (preferably 1 hour) after hot water extraction is finished, carrying out refrigerated centrifugation, taking supernate, namely crude polysaccharide extracting solution, carrying out rotary evaporation and concentration to a certain volume, adding ethanol solution (preferably 95% ethanol solution) to the final ethanol volume fraction, standing overnight, carrying out refrigerated centrifugation on sample solution, taking precipitate, adding a proper amount of distilled water to completely dissolve the precipitate, carrying out reduced pressure evaporation, completely evaporating residual ethanol, concentrating, and carrying out freeze drying to obtain algal polysaccharide;
(b) the algal polysaccharide enzymolysis method comprises the following steps: preparing a seaweed polysaccharide solution with the mass concentration of 2-7% (preferably 5%) by using distilled water, adding glucanase with the mass of 2-5% (preferably 3.5%) by mass of the seaweed polysaccharide, reacting for 1-3 h (preferably 2h) under the conditions that the pH value is 4.8 and the temperature is 48 ℃, standing, cooling, and concentrating by reduced pressure evaporation to a certain concentration for later use; selecting a dialysis bag with the pore size of 500Da, filling the dialysis bag with concentrated liquid flow for dialysis for 12-36 h (preferably 24h), and standing overnight; repeating the steps for multiple times, decompressing and concentrating the dialyzate, and freeze-drying to obtain the algal polysaccharide enzymolysis product.
In the step (5) of the present invention, the preservative may be selected from preservatives commonly used in the art, such as benzyl alcohol, imidazolidinyl urea, methyl paraben, and the like, in the present invention, a mixture of benzyl alcohol, imidazolidinyl urea, and methyl paraben is preferably used as the preservative, and the added mass of the preservative is 0.3 to 0.4% of the mass of the nanoemulsion, and most preferably 0.2% of benzyl alcohol, 0.1% of imidazolidinyl urea, and 0.05% of methyl paraben are used as the preservative.
In step (5), the high-pressure homogenization conditions are as follows: and circularly homogenizing for 5-15 times by a high-pressure homogenizer under the conditions of 70-150 MPa pressure and 75-90 ℃, using a cooling device at the outlet of the high-pressure homogenizer to ensure that the temperature of the mixed liquid at the outlet section of the high-pressure homogenizer is not more than 90 ℃, and obtaining the nano emulsion after homogenization.
The advantages and the beneficial effects of the invention are as follows:
(1) according to the invention, the seaweed polysaccharide is subjected to enzymolysis treatment and then mixed with phospholipid to form the compound emulsifier, and the compound emulsifier has better emulsibility and moisture retention.
Specifically, algal polysaccharides have excellent colloidal properties and also have a certain moisture-retaining property. After the seaweed polysaccharide is subjected to enzymolysis treatment by glucanase, the molecular weight of the polysaccharide is reduced by the breakage of glycosidic bonds, the viscosity of the solution is reduced, and a hydrophobic area and an active site of the seaweed polysaccharide can be exposed, so that the emulsifying activity and the antioxidant activity of the seaweed polysaccharide are improved. The phospholipid is a natural amphoteric emulsifier, has good moisturizing capability and emulsifying capability, and the formed emulsion has good stability. The seaweed polysaccharide enzymolysis product is mixed with phospholipid to obtain a compound emulsifier, and the formed emulsion contains macromolecular polysaccharide serving as an interface stabilizer and small-molecular phospholipid distributed among macromolecules, so that the surface activation energy can be effectively reduced. The hydrophilic groups on the algal polysaccharide enzymolysis product have different structures with the hydrophilic groups of the phospholipid, so that different active ingredients can be stabilized, and the two are compounded for use, so that the emulsification advantages are complementary and the good moisturizing effect is achieved.
(2) The invention mixes arbutin, ascorbyl glucoside and nicotinamide according to a certain proportion to be used as an oil phase, and has the whitening effect.
Specifically, arbutin is a natural active substance derived from green plants, can rapidly permeate into skin, can effectively inhibit the activity of tyrosinase in the skin and block the formation of melanin while not influencing the cell proliferation concentration, accelerates the decomposition and excretion of the melanin by directly combining with the tyrosinase, thereby reducing the pigmentation of the skin, removing color spots and freckles, and does not generate toxic, irritant, sensitizing and other side effects on melanocytes, and also has the effects of sterilization and inflammation diminishing. The reduced glutathione is tripeptide containing gamma-amido bond and sulfhydryl, consists of glutamic acid, cysteine and glycine, has antioxidation and integrated detoxification functions, is rich in reduced glutathione in organisms, can correct the imbalance of acetylcholine and cholinesterase, has an antiallergic effect, can prevent skin aging and pigmentation, reduces the formation of melanin, and enables the skin to be glossy. Nicotinamide is a derivative of vitamin B3, is involved in the transport of melanin and accelerates the rate of melanosome movement in melanocytes, inhibiting the transport of melanin that has been formed to epidermal keratinocytes, and thus leading to a reduction in melanin in the skin. The three mechanisms respectively achieve the whitening effect by inhibiting the activity of tyrosinase, reducing each intermediate in the process of forming melanin and inhibiting the formed melanin from transferring to epidermal keratinocytes.
(3) According to the invention, the tea polyphenol is added into the emulsion, so that the whitening effect of the emulsion can be increased, and the effect of stabilizing the emulsion can be achieved.
In particular, from a cosmetic point of view, in addition to the above three mechanisms to achieve whitening effects, endothelin antagonists are now a new whitening strategy. Tea polyphenol is an endothelin antagonist, has an action mechanism different from the inhibition of tyrosinase activity, and achieves the effects of whitening and removing freckles by inhibiting the regulation and control of endothelin on the proliferation of melanocytes. Under the action of tea polyphenols, endothelin cannot be linked to the receptor sites on melanocortin cells, and therefore there is no additional melanin formation. In addition, the tea polyphenol can interact with the algal polysaccharide enzymolysis product through hydrogen bonds, electrostatic interaction and the like, and the addition of the tea polyphenol can change the secondary structure of the algal polysaccharide enzymolysis product, so that the emulsifying property of the algal polysaccharide enzymolysis product is improved.
(IV) detailed description of the preferred embodiment
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
example 1: preparation of algal polysaccharide enzymolysis product
1. The extraction method of algal polysaccharide comprises the steps of cleaning algae, controlling water, placing the algae in an oven for drying at 60 ℃, crushing, taking 1kg of algae powder, adding 2L 95% ethanol solution for soaking and degreasing, standing overnight, taking the degreased algae powder, adding distilled water according to the material-liquid ratio of 1kg: 10L, carrying out water bath at 95 ℃ for 2h, cooling after hot water extraction is finished, standing for 1h, carrying out refrigerated centrifugation for 10min (rotation speed 10000rpm and temperature 4 ℃), taking supernatant fluid, namely crude polysaccharide extract, carrying out rotary evaporation and concentration to 2L, adding 95% ethanol solution until the volume fraction of final ethanol is 30%, standing overnight, carrying out refrigerated centrifugation on sample fluid for 10min (rotation speed 10000rpm and temperature 4 ℃), taking precipitate, adding a small amount of distilled water to completely dissolve the precipitate, carrying out reduced pressure evaporation and completely evaporating residual ethanol, concentrating to 20m L, and carrying out refrigerated drying to obtain algal polysaccharide.
2. The algal polysaccharide enzymolysis method comprises the steps of preparing 5% algal polysaccharide solution by using distilled water, adding glucanase (purchased from Ningxia Seisakusho industries group Co., Ltd.) with the mass of 3.5% of algal polysaccharide, reacting for 2 hours at the temperature of 48 ℃ under the condition that the pH value is 4.8, standing, cooling, carrying out reduced pressure evaporation and concentration to 4% for later use, selecting a dialysis bag with the aperture size of 500Da, filling 20m L enzymolysis reaction liquid with 4% of soluble solid matter into the dialysis bag, carrying out running water dialysis for 24 hours respectively, standing overnight, repeating for multiple times, carrying out reduced pressure concentration on the dialysate to 10m L, and carrying out freeze drying to obtain the algal polysaccharide enzymolysis product.
Example 2:
(1) weighing 20g hydrogenated soybean oil (purchased from Hezhong Biochemical manufacturing Co., Ltd., Wuhan City) and heating to 85 ℃ to obtain a liquid oil phase I;
(2) weighing 4g of arbutin (purchased from Xian Lutian biotechnology, Inc.), 6g of ascorbyl glucoside (purchased from Xian Wanfang biotechnology, Inc.) and 1g of nicotinamide (purchased from Henan Datang chemical Co., Ltd.) according to the mass ratio of 4: 6: 1, and mixing the three substances to obtain the composite whitening active substance;
(3) weighing 6g of the composite whitening active substance and the liquid oil phase I in a mass ratio of 0.30: 1, adding into the liquid oil phase I obtained in the step (1), and uniformly mixing to obtain a liquid oil phase II;
(4) according to the mass ratio of 0.2: weighing 30g of algal polysaccharide enzymolysis product, 15g of phospholipid and 150g of distilled water according to the ratio of 0.1: 1, heating to 75-85 ℃, and uniformly mixing to obtain a liquid water phase;
(5) according to the mass ratio of 25: 150: weighing 25g of the liquid oil phase II obtained in the step (3), 150g of the liquid water phase obtained in the step (4) and 1g of tea polyphenol, mixing and stirring the liquid oil phase II, the liquid water phase and the tea polyphenol uniformly to obtain a mixed solution, circularly homogenizing the mixed solution for 5 times by a high-pressure homogenizer under the conditions of 150MPa pressure and 90 ℃, using a cooling device at the outlet of the high-pressure homogenizer to ensure that the temperature of the mixed solution at the outlet section of the high-pressure homogenizer is not more than 90 ℃, and obtaining the nano emulsion after homogenization is finished; cooling the obtained nano emulsion to room temperature, and adding 0.2% of benzyl alcohol, 0.1% of imidazolidinyl urea and 0.05% of methyl paraben serving as preservatives by taking the mass of the emulsion as 100% to obtain the emulsion with the effects of whitening and moisturizing.
Example 3:
(1) weighing 15g hydrogenated soybean oil (purchased from Hezhong Biochemical manufacturing Co., Ltd., Wuhan City) and heating to 85 ℃ to obtain a liquid oil phase I;
(2) weighing 1g of arbutin (purchased from Xian Lutian biotechnology, Inc.), 1.5g of ascorbyl glucoside (purchased from Xian Wanfang biotechnology, Inc.) and 0.5g of nicotinamide (purchased from Henan Datang chemical engineering, Inc.) according to the mass ratio of 2: 3: 1, and mixing the three substances to obtain the composite whitening active substance;
(3) weighing 2.25g of the composite whitening active substance and the liquid oil phase I according to the mass ratio of 0.15: 1, adding into the liquid oil phase I obtained in the step (1), and uniformly mixing to obtain a liquid oil phase II;
(4) according to the mass ratio of 0.08: weighing 12g of algal polysaccharide enzymolysis product, 7.5g of phospholipid and 150g of distilled water according to the ratio of 0.05: 1, heating to 75-85 ℃, and uniformly mixing to obtain a liquid water phase;
(5) according to the mass ratio of 15: 120: weighing 15g of the liquid oil phase II obtained in the step (3), 120g of the liquid water phase obtained in the step (4) and 1g of tea polyphenol, mixing and stirring the liquid oil phase II, the liquid water phase and the tea polyphenol uniformly to obtain a mixed solution, circularly homogenizing the mixed solution for 5 times by a high-pressure homogenizer under the conditions of 150MPa pressure and 90 ℃, using a cooling device at the outlet of the high-pressure homogenizer to ensure that the temperature of the mixed solution at the outlet section of the high-pressure homogenizer is not more than 90 ℃, and obtaining the nano emulsion after homogenization is finished; cooling the obtained nano emulsion to room temperature, and adding 0.2% of benzyl alcohol, 0.1% of imidazolidinyl urea and 0.05% of methyl paraben serving as preservatives by taking the mass of the emulsion as 100% to obtain the emulsion with the effects of whitening and moisturizing.
Example 4:
(1) weighing hydrogenated soybean oil (purchased from Synzhou Biochemical manufacturing Co., Ltd., Wuhan City) 20g, and heating to 85 deg.C to obtain liquid oil phase I
(2) Weighing 1.6g of arbutin (purchased from Xian Lutian biotechnology, Inc.), 4.8g of ascorbyl glucoside (purchased from Xian Wanfang biotechnology, Inc.) and 0.8g of nicotinamide (purchased from Henan Datang chemical engineering, Inc.) according to the mass ratio of 2: 6: 1, and mixing the three substances to obtain a composite whitening active substance;
(3) weighing 4g of the composite whitening active substance and the liquid oil phase I in a mass ratio of 0.2: 1, adding into the liquid oil phase I obtained in the step (1), and uniformly mixing to obtain a liquid oil phase II;
(4) according to the mass ratio of 0.08: weighing 12g of algal polysaccharide enzymolysis product, 15g of phospholipid and 150g of distilled water according to the ratio of 0.1: 1, heating to 75-85 ℃, and uniformly mixing to obtain a liquid water phase;
(5) according to the mass ratio of 25: 140: weighing 25g of the liquid oil phase II obtained in the step (3), 140g of the liquid water phase obtained in the step (4) and 1g of tea polyphenol, mixing and stirring the liquid oil phase II, the liquid water phase and the tea polyphenol uniformly to obtain a mixed solution, circularly homogenizing the mixed solution for 5 times by a high-pressure homogenizer under the conditions of 150MPa pressure and 90 ℃, using a cooling device at the outlet of the high-pressure homogenizer to ensure that the temperature of the mixed solution at the outlet section of the high-pressure homogenizer is not more than 90 ℃, and obtaining nano emulsion after homogenization is finished; cooling the obtained nano emulsion to room temperature, and adding 0.2% of benzyl alcohol, 0.1% of imidazolidinyl urea and 0.05% of methyl paraben serving as preservatives by taking the mass of the emulsion as 100% to obtain the emulsion with the effects of whitening and moisturizing.
Example 5: and (3) testing the emulsion performance:
(1) tyrosinase inhibition rate determination experimental method:
adding a sample system, namely preparing Phosphate Buffer Solution (PBS) with the pH value of 6.8, preparing tyrosinase phosphate buffer solution with the concentration of 200U/m L (operating and storing in ice water bath), preparing L-tyrosine buffer solution with the concentration of 2.5 mmol/L, taking 1.5m L L-tyrosine buffer solution, 1.5m L PBS solution and 1m L of the emulsion with the whitening and moisturizing effects prepared in the embodiment, mixing, preserving the mixture in water bath at 37 ℃ for 10min, adding 1m L tyrosinase phosphate buffer solution, reacting for 10min, and measuring the light absorption value at 475 nm.
The sample system without adding sample comprises preparing Phosphate Buffer Solution (PBS) with pH of 6.8, tyrosinase phosphate buffer solution with concentration of 200U/m L (operating and storing in ice water bath), L-tyrosine buffer solution with concentration of 2.5 mmol/L, mixing 1.5m L L-tyrosine buffer solution, 1.5m L PBS solution and 1m L deionized water, preserving heat in water bath at 37 ℃ for 10min, adding 1m L tyrosinase phosphate buffer solution, reacting for 10min, and measuring absorbance at 475 nm.
The inhibition of tyrosinase was calculated as follows:
inhibition ratio (A-B)/A × 100%
Wherein A is the absorbance value of the system without the sample, and B is the absorbance value of the system after the sample is added.
The test results are shown in Table 1.
(2) The stability test indexes are as follows:
a. heat resistance. After the whitening and moisturizing emulsion is stored at 40 ℃ for 15 days, whether the characteristics and the color of the whitening and moisturizing emulsion are obviously different from those before the test or not, whether the phenomena of layering and oil floating exist or not is observed visually, and if the phenomena are not obviously different, the heat resistance of the emulsion product is better.
b. Cold resistance. After the whitening and moisturizing emulsion is stored at 0 ℃ for 15 days, whether the characters and colors of the whitening and moisturizing emulsion are obviously different from those before the test or not, whether the phenomena of layering and oil floating exist or not is observed visually, and if the phenomena of layering and oil floating do not exist, the cold resistance of the emulsion product is better.
c. And (4) cold and hot circulation. After cold-hot circulation alternation experiments (standing at 40 ℃ for 15 days, then at 0 ℃ for 15 days, and carrying out circulation treatment for 3 times), the whitening and moisturizing emulsion is observed visually to find whether the emulsion has obvious differences in properties and colors before the experiments, and whether the emulsion has the phenomena of layering and oil floating, and if the emulsion has no obvious differences, the emulsion product has good cold resistance.
The test results are shown in Table 1.
(3) And (4) moisture retention performance test: applying the lotion on hand for 15min, measuring skin water content change within 30min with skin moisture tester (Haiyue skin tester), measuring at the same position of hand for 3 times, and averaging. Before the whitening and moisturizing emulsion is not applied, the moisture content of the skin at the same position of the hand is basically maintained at 33.6% after 30 min.
TABLE 1
Claims (3)
1. A preparation method of an emulsion with whitening and moisturizing effects comprises the following steps:
(1) weighing hydrogenated soybean oil, and heating to 75-85 ℃ to obtain a liquid oil phase I;
(2) weighing arbutin, ascorbyl glucoside and nicotinamide according to the mass ratio of 2-4: 3-6: 1, and mixing the three substances to obtain a composite whitening active substance;
(3) adding the composite whitening active substance into the liquid oil phase I obtained in the step (1), and uniformly mixing to obtain a liquid oil phase II; wherein the mass ratio of the composite whitening active substance to the liquid oil phase I is 0.15-0.30: 1;
(4) according to the mass ratio of 0.08-0.2: weighing the algal polysaccharide enzymolysis product, phospholipid and distilled water according to the ratio of 0.05-0.1: 1, heating to 75-85 ℃, and uniformly mixing to obtain a liquid water phase;
(5) according to the mass ratio of 15-25: 120-150: 1, weighing the liquid oil phase II obtained in the step (3), the liquid water phase obtained in the step (4) and tea polyphenol, mixing and stirring uniformly to obtain a mixed solution, carrying out high-pressure homogenization on the mixed solution in a high-pressure homogenizer to obtain nano emulsion, and ensuring that the temperature of the mixed solution at an outlet section of the high-pressure homogenizer is not more than 90 ℃; cooling the obtained nano emulsion to room temperature, and adding a proper amount of preservative to obtain the emulsion with whitening and moisturizing effects;
the preparation method of the algal polysaccharide enzymolysis product comprises the following specific operation steps:
(a) the algal polysaccharide extraction method comprises the steps of cleaning algae, drying and crushing to obtain algal powder, soaking and degreasing the algal powder in 95% ethanol solution by volume, standing overnight, adding distilled water into the degreased algal powder according to the material-liquid ratio of 1kg to 8-12L, carrying out water bath at 80-100 ℃ for 1-3 h, cooling and standing for 0.5-1.5 h after hot water extraction is finished, carrying out refrigerated centrifugation, taking supernate, namely polysaccharide crude extract, carrying out rotary evaporation and concentration to a certain volume, adding the ethanol solution until the final ethanol volume fraction is 30%, standing overnight, carrying out refrigerated centrifugation on sample liquid, taking precipitate, adding a proper amount of distilled water to completely dissolve the precipitate, carrying out reduced pressure evaporation, completely evaporating residual ethanol, concentrating, and carrying out freeze drying to obtain algal polysaccharide;
(b) the algal polysaccharide enzymolysis method comprises the following steps: preparing a seaweed polysaccharide solution with the mass concentration of 2-7% by using distilled water, adding glucanase with the mass concentration of 2-5% by mass of the seaweed polysaccharide, reacting for 1-3 h under the conditions that the pH value is 4.8 and the temperature is 48 ℃, standing, cooling, and carrying out reduced pressure evaporation and concentration to a certain concentration for later use; selecting a dialysis bag with the aperture size of 500Da, filling the dialysis bag into concentrated liquid flow for dialysis for 12-36 h, and standing overnight; repeating the steps for multiple times, decompressing and concentrating the dialyzate, and freeze-drying to obtain the algal polysaccharide enzymolysis product.
2. The method of claim 1, wherein: in the step (5), the preservative is a mixture of benzyl alcohol, imidazolidinyl urea and methyl paraben, and the adding mass of the preservative is 0.3-0.4% of the mass of the nano emulsion.
3. The method of claim 1, wherein: in the step (5), the high-pressure homogenizing condition is as follows: and circularly homogenizing for 5-15 times by a high-pressure homogenizer under the conditions of 70-150 MPa pressure and 75-90 ℃, using a cooling device at the outlet of the high-pressure homogenizer to ensure that the temperature of the mixed liquid at the outlet section of the high-pressure homogenizer is not more than 90 ℃, and obtaining the nano emulsion after homogenization.
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| JPS5929607A (en) * | 1982-08-10 | 1984-02-16 | Iwasekenjirou Shoten:Kk | Oil-in-water type emulsified composition for external skin use |
| GB2529962A (en) * | 2013-05-30 | 2016-03-09 | Suzhou Sciscape Bio Pharmaceutical Technology Co Ltd | Multi-functional composition and preparation method and application thereof |
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| CN108354864A (en) | 2018-08-03 |
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