CN111514038A - Preparation method and application of tetrahydrocurcumin-loaded microcapsule - Google Patents
Preparation method and application of tetrahydrocurcumin-loaded microcapsule Download PDFInfo
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- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/11—Encapsulated compositions
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- A61K8/00—Cosmetics or similar toiletry preparations
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
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- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
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- A—HUMAN NECESSITIES
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- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/84—Products or compounds obtained by lyophilisation, freeze-drying
Abstract
The invention discloses a preparation method of a tetrahydrocurcumin-loaded microcapsule and application of the tetrahydrocurcumin-loaded microcapsule in cosmetics. The preparation method comprises the following steps: the preparation method comprises the steps of self-assembling and preparing the amphiphilic octenyl succinic acid short glucan nano micelle in an aqueous solution by adopting a direct dissolution method, and embedding tetrahydrocurcumin to prepare the loaded tetrahydrocurcumin microcapsule by taking the amphiphilic octenyl succinic acid short glucan chain nano micelle as a wall material. The invention provides the preparation method of the tetrahydrocurcumin microcapsule, which is simple and convenient to operate, low in cost and capable of obviously improving the stability and the sustained release effect of the tetrahydrocurcumin, and has the advantages of long action time and high absorption efficiency in cosmetics.
Description
Technical Field
The invention relates to a preparation method of tetrahydrocurcumin microcapsules, in particular to a preparation method of tetrahydrocurcumin microcapsules and application of the tetrahydrocurcumin microcapsules in cosmetics, and belongs to the field of daily chemical industry.
Background
With the increase of the economic level, the requirements on the functional ingredients of the cosmetics are increased. The developed and found efficacy components of the star comprise niacinamide, arbutin, hyaluronic acid, VC and the like, and the tetrahydrocurcumin is a natural functional whitening raw material and also has multi-aspect and multi-level effects. It has potent activity of inhibiting tyrosinase, and its whitening effect is superior to arbutin. The tetrahydrocurcumin has extremely excellent antioxidant effect, active oxygen induces a series of reactions on the surface of skin, such as tissue damage, cell aging and the like, and the tetrahydrocurcumin can effectively improve the damage of free radicals to the skin and protect the skin. In addition, ultraviolet radiation can destroy the skin phospholipid layer to cause skin inflammation, the inflammation is expressed as erythema, if the inflammation is not relieved in time, pigmentation can be caused, real melanin is gradually formed, the skin is blackened, and the tetrahydrocurcumin can effectively resist the skin inflammation and prevent the skin from generating redness and swelling and erythema. Tetrahydrocurcumin is widely used in various skin care products with whitening, freckle removing and oxidation resistance, such as cream, emulsion and essence products, due to the excellent performance of tetrahydrocurcumin. In addition, tetrahydrocurcumin is used as a novel pharmaceutical raw material and an intermediate for its antitumor and antiatherosclerotic effects, and is also a new effect as a food additive.
However, the existing tetrahydrocurcumin has the problems of poor stability, low bioavailability and the like, and has certain limit in the aspects of development and application. The microcapsule is coated in the microcapsule, so that the stability and the bioavailability of the microcapsule are improved, and the application range of the microcapsule can be greatly expanded. And the tetrahydrocurcumin microcapsule has a slow release effect, can greatly improve the action time and the action effect, and has certain improvement on the effects of oxidation resistance, whitening, sun protection and the like.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the existing tetrahydrocurcumin has the problems of poor stability, low bioavailability and the like.
In order to solve the technical problems, the invention provides a preparation method of a tetrahydrocurcumin-loaded microcapsule, which is characterized by comprising the following steps: the preparation method comprises the steps of self-assembling and preparing the amphiphilic octenyl succinic acid short glucan nano micelle in an aqueous solution by adopting a direct dissolution method, and embedding tetrahydrocurcumin to prepare the loaded tetrahydrocurcumin microcapsule by taking the amphiphilic octenyl succinic acid short glucan chain nano micelle as a wall material.
Preferably, the preparation method specifically comprises the following steps: preparing octenyl succinic acid short chain glucan nano particle powder into an aqueous solution, mixing the aqueous solution with a tetrahydrocurcumin ethanol solution, heating at 37-45 ℃ for 60-70min to fully gelatinize and disperse the mixture, performing rotary evaporation at 38-45 ℃ for 30-50min to remove ethanol, and finally performing freeze drying for 48-72 h.
More preferably, the concentration of the aqueous solution of the octenyl succinic acid short-chain glucan nanoparticle powder is 10 mg/mL; the concentration of the tetrahydrocurcumin ethanol solution is 5 mg/mL; the mass ratio of the octenyl succinic acid short-chain glucan nanoparticle powder to the tetrahydrocurcumin is 3: 1.
More preferably, the preparation method of the octenyl succinic acid short-chain glucan nanoparticle powder comprises the following steps: dissolving octenylsuccinic acid short-chain glucan powder in a phosphate buffer solution, stirring, keeping the temperature at 37-55 ℃ for 6-12h, cooling to room temperature, washing with alcohol for 2-3 times, precipitating, washing with water for 2-3 times, and finally freeze-drying for 48-72 h.
Further, the pH value of the phosphate buffer solution is 7.4; the alcohol washing adopts absolute ethyl alcohol.
Further, the preparation method of the octenyl succinic acid short-chain glucan powder comprises the following steps: preparing short-chain glucan into an aqueous solution, stirring and gelatinizing at 90-100 ℃ for 30-50min, and adjusting the pH value to 8.0-8.5 by using an alkali solution after gelatinizing is finished; dispersing octenyl succinic anhydride in absolute ethyl alcohol, reducing the temperature to 50-68 ℃, and adjusting the pH value to 8.5-9.0 by using alkali solution; adding octenyl succinic anhydride solution into short-chain dextran solution, continuously stirring for 8-10h, adjusting pH to 6.5-7.0 with acid solution, washing with alcohol for 2-3 times, precipitating, cooling the precipitate at 4 deg.C for 8-12h, and freeze drying for 48-72 h.
Further, the concentration of the short-chain glucan solution is 50 g/L; NaOH is adopted as the alkali solution; adopting HCl as an acid solution; absolute ethyl alcohol is adopted for alcohol washing; the mass ratio of the octenyl succinic anhydride solution to the short-chain glucan solution is 4-1: 1.
Further, the preparation method of the short-chain glucan comprises the following steps: mixing waxy corn starch slurry with phosphate buffer solution, vigorously stirring in boiling water at 100 deg.C for about 30-50min for gelatinization, adding pullulanase, incubating at pH of 8-9 and 55-65 deg.C for 6-8 hr, centrifuging for 2-5min, and freeze drying for 48-72 hr.
Further, the mass ratio of the waxy corn starch slurry to the phosphate buffer solution is 1: 1; the pH value of the phosphate buffer solution is 5.0; the enzyme activity of the pullulanase is 1000 ASPU/g.
The invention also provides application of the microcapsule prepared by the preparation method of the microcapsule loaded with tetrahydrocurcumin in cosmetics, which is characterized in that raw materials of the cosmetics comprise the following components in percentage by weight:
the balance of deionized water.
Preferably, the emulsifier is at least one of stearic acid, steareth-21 and sodium stearyl glutamate; the composite lipid material is at least one of glycerol tri (ethyl hexanoate), polydimethylsiloxane, stearyl alcohol, squalane, oleate and butanediol; the pH regulator is sodium hydroxide or citric acid; the water phase material is at least one of glycerol, sodium hyaluronate, glycosyl trehalose and carbomer; the preservative is at least one of methyl hydroxybenzoate, propyl hydroxybenzoate and phenoxyethanol.
Preferably, the preparation method of the cosmetic comprises the following steps: preparing stearyl glutamate sodium, sodium hydroxide, citric acid glycerol, sodium hyaluronate, glycosyl trehalose and carbomer into a water phase system, preparing stearic acid, steareth-21, glycerol tri (ethyl hexanoate) ester, polydimethylsiloxane, stearyl alcohol, squalane, oleate, butanediol, methyl hydroxybenzoate, propyl hydroxybenzoate and phenoxyethanol into an oil phase system, and respectively heating to 70-80 ℃; slowly adding the water phase system into the oil phase system, homogenizing at 80-95 deg.C until the paste turns into milk white, stirring for 3-5min, stopping heating, stirring at 40 deg.C, adding the microcapsule, stirring, and cooling to room temperature.
The invention provides the preparation method of the tetrahydrocurcumin microcapsule, which is simple and convenient to operate and low in cost, has obviously improved stability and sustained release effect on the tetrahydrocurcumin, and solves the problems of reduced experience and use effect of people.
Compared with the prior art, the invention has the beneficial effects that:
the invention selects waxy corn starch as the raw material for preparing the microcapsule wall material, and has the advantages of wide source, mature raw material preparation method, low price, easy obtainment, safety, no toxicity and the like in production. Structurally, more than 95% of waxy corn starch is branched chain, 5% of waxy corn starch is straight chain, and in order to better utilize the spiral cavity structure characteristic of SGC, SGC is obtained by a pullulanase enzymolysis method.
The food-grade amphiphilic octenyl succinic acid short glucan is safe and non-toxic, has high acceptance, is internally hydrophobic and externally hydrophilic, and is commonly used for embedding the flavor essence. The amphiphilic octenyl succinic acid short glucan chain polymer has good embedding performance and is a microcapsule wall material with good performance.
According to the invention, waxy corn starch is subjected to enzymolysis to form short-chain glucan to prepare amphiphilic octenyl succinic acid short glucan, then the amphiphilic octenyl succinic acid short glucan is used as a wall material to embed tetrahydrocurcumin to prepare tetrahydrocurcumin microcapsules, and finally the tetrahydrocurcumin microcapsules are applied to the preparation of cosmetics, so that the action time of the tetrahydrocurcumin in the cosmetics is prolonged, the action effect of the tetrahydrocurcumin is enhanced, and the effects of whitening, antioxidation and skin protection are stronger.
Drawings
FIG. 1 shows OSA (A), SGC (B), OSA0.25-SGC(C)，OSA0.5SGC (D) and OSA1.0-a comparison of hydrogen nuclear magnetic resonance spectra of sgc (e);
FIG. 2 is an OSA with different degrees of substitution0.25-SGC(A)，OSA0.5SGC (B) and OSA1.0-a comparison of TEM images of sgc (c);
FIG. 3 is a comparative graph of SEM images of the microcapsule (A) prepared in example 1, the microcapsule (B) prepared in example 2, and the microcapsule (C) prepared in example 3;
FIG. 4 is a schematic diagram of a preparation method provided by the present invention.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
The specifications of the raw materials used in examples 1-3 and the manufacturer information are as follows: waxy corn starch is available from national starch chemistry, ltd; pullulanase is derived from Shanghai-derived leaf Biotechnology, Inc.; other reagents were analytically pure and were purchased from Shanghai Tantake Technique, Inc.
In examples 1 to 3, the degree of substitution was measured by the following method: NMR is a common method for determining the degree of octenyl succinate substitution of short glucan chains. The experiment was performed by hydrogen spectroscopy (Brook, Steffisburg, switzerland) at 600MHZ, weighing 20mg OSA, SGC and OSA-SGC nanoparticles, respectively, into a nuclear magnetic tube, and adding 0.7mL deuterated dimethyl sulfoxide (DMSO-d6) containing 0.5 wt% lithium bromide. The mixture was then heated at 80 ℃ to dissolve those nanoparticles, and finally 20mg of deuterated trifluoroacetic acid (TFA-d1) was added to the solution. The degree of substitution is calculated as follows:
in the formula I0.89Indicating CH in OSA3Integral of the signal peak, Iα-1,4Represents the integral of the signal peak at 5.11ppm for the proton on the carbon atom to which α - (1 → 4) is attached, Iα-1,6Denotes the integral of the peak of the proton signal at the carbon atom to which α - (1 → 6) is attached, Ir-eCorresponding to the reducing strand end. I isr-eBeing at the end of the reducing chains of inner portions α and β1Integration by HNMR was about 4.28ppm and 4.91ppm in the short glucan chains, respectively.
Wall material OSA-SGC was observed using a Brookfield Tecnai G2F 30-TWIN transmission electron microscope in Germany with an acceleration voltage of 200 kV. The OSA-SGC nanoparticle dry powder was formulated as a 1% by mass solution and sonicated at room temperature for 10 minutes, then dropped onto a copper mesh with a carbon support film, and then freeze dried for measurement. The sample remains sterile and transparent.
The tetrahydrocurcumin microcapsules are observed by a scanning electron microscope. Adding 10mL of ultrapure water into a 0.1mg sample, carrying out ultrasonic treatment for 10min, uniformly dispersing, placing a drop of sample in the middle of a beaker on a sample table attached with conductive adhesive, carrying out gold spraying treatment on the sample, and then adjusting to an optimum multiple under the conditions of current 3mA and acceleration voltage 15kV to observe the micro-morphology.
Example 1
A preparation method of tetrahydrocurcumin microcapsules and application of the tetrahydrocurcumin microcapsules in cosmetics comprise the following specific steps:
(1) the preparation method of the short-chain glucan comprises the following steps:
a certain mass of waxy corn starch (15g/mL) slurry (100mL phosphate buffer, pH 5.0) was stirred vigorously in boiling water at 100 deg.C for about 30min to gelatinize. Pullulanase (1000ASPU/g) was then added and incubated at 55 ℃ at pH 8 for 6h and centrifuged at 1300 × g for 3 min. And finally, carrying out freeze drying for 48 hours to obtain SGC powder.
(2) The preparation method of the octenyl succinic acid short-chain glucan comprises the following steps:
5g of SGC powder is prepared into a 50g/L SGC aqueous solution by using 100mL of distilled water, then stirred and gelatinized for 30min at 90 ℃, and after the gelatinization is finished, 0.1mol/L NaOH is added to keep the pH value of the solution at 8.0. Octenyl succinic anhydride was then dispersed in about 2mL of absolute ethanol and the sample temperature was lowered to 50 ℃ and pH was maintained at 8.5 using NaOH, and the OSA solution was added to the sample with continuous stirring for 8 h. OSA was added in an amount of 25% by dry weight of SGC powder and was designated OSA0.25-SGC. Adjusting pH to 6.5 with 0.1mol/LHCl, washing with 99.7% anhydrous ethanol for 2 times, precipitating, cooling at 4 deg.C for 8 hr, and lyophilizing for 48 hr to obtain OSA0.25-SGC powder.
(3) The preparation method of the octenyl succinic acid short-chain glucan nano particle powder comprises the following steps:
get OSA0.25-SGC powder, dissolved in phosphate buffer solution at pH 7.4, stirred, maintained at 37 ℃ for 6h to prepare OSA0.25-SGC nanoparticle solution, which is cooled to room temperature. And then the precipitate is precipitated after being washed with absolute ethyl alcohol for 2 times, and is washed with water for 2 times. Then freeze-drying for 48h to obtain OSA0.25-SGC nanoparticle powder.
(4) The preparation method of the tetrahydrocurcumin microcapsule comprises the following steps:
preparing 10mg/mL octenyl succinic acid short-chain glucan aqueous solution and 5mg/mL tetrahydrocurcumin ethanol solution, heating at 37 ℃ for 60min to fully gelatinize and disperse, performing rotary evaporation at 38 ℃ for 30min to remove ethanol, and freeze-drying for 48h to obtain the tetrahydrocurcumin microcapsule.
(5) Preparation of cosmetics containing tetrahydrocurcumin microcapsules:
weighing the following components in percentage by weight: 0.5% of tetrahydrocurcumin microcapsule, 5% of emulsifier, 5% of composite lipid material, 0.1% of pH regulator, 3% of water phase material, 0.1% of preservative and 86.3% of deionized water.
Wherein the oil-in-water emulsifier is stearic acid, steareth-21 and sodium stearyl glutamate. The composite lipid material is glycerol tri (ethyl caproate), polydimethylsiloxane, stearyl alcohol, squalane, oleate and butanediol. The pH regulator is sodium hydroxide and citric acid. The water phase material is glycerol, sodium hyaluronate, glycosyl trehalose, and carbomer. The antiseptic is methyl hydroxybenzoate, propyl hydroxybenzoate, and phenoxyethanol.
After the preparation of each phase was completed, the phases were heated to 70 ℃. Slowly adding the prepared water phase into the oil phase system, homogenizing (3000r/min) at 80 deg.C until the paste turns into milk white, stirring for 3min, stopping heating, stirring to 40 deg.C under reduced speed, adding tetrahydrocurcumin microcapsule, stirring, and cooling to room temperature.
Example 2
A preparation method of tetrahydrocurcumin microcapsules and application of the tetrahydrocurcumin microcapsules in cosmetics comprise the following specific steps:
(1) the preparation method of the short-chain glucan comprises the following steps:
a certain mass of waxy corn starch (15g/mL) slurry (100mL phosphate buffer, pH 5.0) was stirred vigorously in boiling water at 100 deg.C for about 40min to gelatinize. Pullulanase (1000ASPU/g) was then added and incubated at 60 ℃ at pH 8.5 for 7h and centrifuged at 1300 × g for 4 min. Finally, the SGC can be obtained by freeze drying for 60 h.
(2) The preparation method of alkenyl succinic acid short-chain glucan comprises the following steps:
5g of SGC powder is taken, 100mL of distilled water is used for preparing 50g/L SGC aqueous solution, stirring is carried out at 90-100 ℃ for gelatinization for 40min, and 0.1mol/L NaOH is added after the gelatinization is completed so as to keep the pH value of the solution at 8.3. Octenyl succinic anhydride was then dispersed in about 2mL of absolute ethanol and the sample temperature was lowered to 60 ℃ and pH was maintained at 8.7 using NaOH, and the OSA solution was added to the sample with continuous stirring for 9 h. OSA was added in an amount of 50% by dry weight of SGC powder and was designated OSA0.5-SGC. Adjusting pH to 6.8 with 0.1mol/L HCl, washing with 99.7% anhydrous ethanol for 3 times, precipitating, cooling at 4 deg.C for 10 hr, and freeze drying for 60 hr to obtain OSA0.5-SGC powder.
(3) The preparation method of the octenyl succinic acid short-chain glucan nano particle dry powder comprises the following steps:
get OSA0.5-SGC powder, dissolved in phosphate buffer solution at pH 7.4, stirred, maintained at 40 ℃ for 10h to prepare OSA0.5-SGC nanoparticle solution, which is cooled to room temperature. Washing with anhydrous alcohol for 2-3 times, precipitating, and washing with water for 2-3 times. Freeze-drying for 48-72h to obtain OSA0.5-SGC nanoparticle powder.
(4) The preparation method of the tetrahydrocurcumin microcapsule comprises the following steps:
preparing 10mg/mL octenyl succinic acid short-chain glucan aqueous solution and 5mg/mL tetrahydrocurcumin ethanol solution, heating at 40 ℃ for 65min to fully gelatinize and disperse, performing rotary evaporation at 40 ℃ for 40min to remove ethanol, and freeze-drying for 60h to obtain the tetrahydrocurcumin microcapsule.
(5) Preparation of cosmetics containing tetrahydrocurcumin microcapsules:
weighing the following components in percentage by weight: 5% of tetrahydrocurcumin microcapsules, 10% of an emulsifier, 10% of a composite lipid material, 1% of a pH regulator, 10% of a water phase material, 1% of a preservative and 63% of deionized water.
Wherein the oil-in-water emulsifier is stearic acid, steareth-21 and sodium stearyl glutamate. The composite lipid material is glycerol tri (ethyl caproate), polydimethylsiloxane, stearyl alcohol, squalane, oleate and butanediol. The pH regulator is sodium hydroxide and citric acid. The water phase material is glycerol, sodium hyaluronate, glycosyl trehalose, and carbomer. The antiseptic is methyl hydroxybenzoate, propyl hydroxybenzoate, and phenoxyethanol.
The phases were heated to 75 ℃ after completion of the preparation. Slowly adding the prepared water phase into the oil phase system, homogenizing (5000r/min) at 90 deg.C until the paste turns to milk white, stirring for 4min, stopping heating, stirring to 40 deg.C under reduced speed, adding tetrahydrocurcumin microcapsule, stirring, and cooling to room temperature.
Example 3
A preparation method of tetrahydrocurcumin microcapsules and application of the tetrahydrocurcumin microcapsules in cosmetics comprise the following specific steps:
(1) the preparation method of the short-chain glucan comprises the following steps:
a certain mass of waxy corn starch (15g/mL) slurry (100mL phosphate buffered saline, pH 5.0) was stirred vigorously in boiling water at 100 deg.C for about 50min to gelatinize. Pullulanase (1000ASPU/g) was then added and incubated at pH 9, 65 ℃ for 8h and centrifuged at 1300 × g for 5 min. Finally, carrying out freeze drying for 72h to obtain the SGC.
(2) The preparation method of the octenyl succinic acid short-chain glucan powder comprises the following steps:
5g of SGC powder is prepared into a 50g/L SGC aqueous solution by using 100mL of distilled water, then stirred and gelatinized for 50min at 100 ℃, and after the gelatinization is finished, 0.1mol/L NaOH is added to keep the pH value of the solution at 8.5. Octenyl succinic anhydride was then dispersed in about 2mL of absolute ethanol and the sample temperature was lowered to 68 ℃ and pH was maintained at 9.0 using NaOH, and the OSA solution was added to the sample with continuous stirring for 10 h. OSA was added in an amount of 100% by dry weight of SGC powder and was designated OSA1.0-SGC. Adjusting pH to 7.0 with 0.1mol/LHCl, washing with 99.7% anhydrous ethanol for 3 times, precipitating, cooling at 4 deg.C for 12 hr, and freeze drying for 72 hr to obtain OSA1.0-SGC powder.
(3) The preparation method of the octenyl succinic acid short-chain glucan nano particle powder comprises the following steps:
get OSA1.0SGC powder, dissolved at pH 7.4Stirring with phosphate buffer solution, maintaining at 55 deg.C for 12 hr to obtain OSA1.0-SGC nanoparticle solution, which is cooled to room temperature. And then, the precipitate was precipitated after washing with absolute ethanol for 3 times, and was washed with water for 3 times. Then freeze-drying for 72h to obtain the OSA1.0-SGC nanoparticle powder.
(4) The preparation method of the tetrahydrocurcumin microcapsule comprises the following steps:
preparing 10mg/mL octenyl succinic acid short-chain glucan aqueous solution and 5mg/mL tetrahydrocurcumin ethanol solution, heating at 45 ℃ for 70min to fully gelatinize and disperse, performing rotary evaporation at 45 ℃ for 50min to remove ethanol, and freeze-drying for 72h to obtain the tetrahydrocurcumin microcapsule.
(5) Preparation of cosmetics containing tetrahydrocurcumin microcapsules:
weighing the following components in percentage by weight: 10% of tetrahydrocurcumin microcapsules, 20% of an emulsifier, 10% of a composite lipid material, 1% of a pH regulator, 15% of a water phase material, 2% of a preservative and 42% of deionized water.
Wherein the oil-in-water emulsifier is stearic acid, steareth-21 and sodium stearyl glutamate. The composite lipid material is glycerol tri (ethyl caproate), polydimethylsiloxane, stearyl alcohol, squalane, oleate and butanediol. The pH regulator is sodium hydroxide and citric acid. The water phase material is glycerol, sodium hyaluronate, glycosyl trehalose, and carbomer. The antiseptic is methyl hydroxybenzoate, propyl hydroxybenzoate, and phenoxyethanol.
After the preparation of each phase was completed, the phases were heated to 80 ℃. Slowly adding the prepared water phase into the oil phase system, homogenizing (7000r/min) at 95 deg.C until the paste turns into milk white, stirring for 5min, stopping heating, stirring to 40 deg.C under reduced speed, adding tetrahydrocurcumin microcapsule, stirring, and cooling to room temperature.
As can be seen from fig. 1, the degree of substitution was increased from 0.112 to 0.286 and 0.342, respectively, by calculation as the octenyl succinic anhydride/dextran short chain ratio was increased from 25% to 50% and 100%, respectively.
FIG. 2 shows that OSA0.25-SGC，OSA0.5SGC and OSA1.0-SGC having a particle size of about15-20, 10-20 and 5-10 nm. The size of the nanomicelles decreases with increasing OSA content, probably due to the increased OSA content, thereby increasing the hydrophobicity and making the core of the micelle denser.
FIG. 3 shows that OSA0.25-SGC，OSA0.5SGC and OSA1.0The surface of the SGC is rough and flaky, probably due to OSA modification.
Claims (12)
1. A preparation method of a tetrahydrocurcumin-loaded microcapsule is characterized by comprising the following steps: the preparation method comprises the steps of self-assembling and preparing the amphiphilic octenyl succinic acid short glucan nano micelle in an aqueous solution by adopting a direct dissolution method, and embedding tetrahydrocurcumin to prepare the loaded tetrahydrocurcumin microcapsule by taking the amphiphilic octenyl succinic acid short glucan chain nano micelle as a wall material.
2. The preparation method of the tetrahydrocurcumin-loaded microcapsule as claimed in claim 1, which comprises the following steps: preparing octenyl succinic acid short chain glucan nano particle powder into an aqueous solution, mixing the aqueous solution with a tetrahydrocurcumin ethanol solution, heating at 37-45 ℃ for 60-70min to fully gelatinize and disperse the mixture, performing rotary evaporation at 38-45 ℃ for 30-50min to remove ethanol, and finally performing freeze drying for 48-72 h.
3. The method for producing tetrahydrocurcumin-loaded microcapsules according to claim 2, wherein the concentration of the aqueous solution of the octenyl succinic acid short-chain glucan nanoparticle powder is 10 mg/mL; the concentration of the tetrahydrocurcumin ethanol solution is 5 mg/mL; the mass ratio of the octenyl succinic acid short-chain glucan nanoparticle powder to the tetrahydrocurcumin is 3: 1.
4. The method for preparing tetrahydrocurcumin-loaded microcapsules of claim 2, wherein said octenyl succinic acid short-chain glucan nanoparticle powder is prepared by: dissolving octenylsuccinic acid short-chain glucan powder in a phosphate buffer solution, stirring, keeping the temperature at 37-55 ℃ for 6-12h, cooling to room temperature, washing with alcohol for 2-3 times, precipitating, washing with water for 2-3 times, and finally freeze-drying for 48-72 h.
5. The method for producing tetrahydrocurcumin-loaded microcapsules according to claim 4, wherein said phosphate buffer has a pH of 7.4; the alcohol washing adopts absolute ethyl alcohol.
6. The method for preparing tetrahydrocurcumin-loaded microcapsules of claim 4, wherein said octenyl succinic acid short-chain glucan powder is prepared by: preparing short-chain glucan into an aqueous solution, stirring and gelatinizing at 90-100 ℃ for 30-50min, and adjusting the pH value to 8.0-8.5 by using an alkali solution after gelatinizing is finished; dispersing octenyl succinic anhydride in absolute ethyl alcohol, reducing the temperature to 50-68 ℃, and adjusting the pH value to 8.5-9.0 by using alkali solution; adding octenyl succinic anhydride solution into short-chain dextran solution, continuously stirring for 8-10h, adjusting pH to 6.5-7.0 with acid solution, washing with alcohol for 2-3 times, precipitating, cooling the precipitate at 4 deg.C for 8-12h, and freeze drying for 48-72 h.
7. The method for producing tetrahydrocurcumin-supporting microcapsules according to claim 6, wherein the concentration of said short-chain glucan solution is 50 g/L; NaOH is adopted as the alkali solution; adopting HCl as an acid solution; absolute ethyl alcohol is adopted for alcohol washing; the mass ratio of the octenyl succinic anhydride solution to the short-chain glucan solution is 4-1: 1.
8. The method for preparing tetrahydrocurcumin-loaded microcapsules of claim 6, wherein said short-chain glucan is prepared by: mixing waxy corn starch slurry with phosphate buffer solution, vigorously stirring in boiling water at 100 deg.C for about 30-50min for gelatinization, adding pullulanase, incubating at pH of 8-9 and 55-65 deg.C for 6-8 hr, centrifuging for 2-5min, and freeze drying for 48-72 hr.
9. The method for preparing tetrahydrocurcumin-loaded microcapsules according to claim 8, wherein the mass ratio of said waxy corn starch slurry to phosphate buffer solution is 1: 1; the pH value of the phosphate buffer solution is 5.0; the enzyme activity of the pullulanase is 1000 ASPU/g.
10. Use of microcapsules loaded with tetrahydrocurcumin as claimed in any of the claims 1 to 9 in cosmetics, characterized in that the raw materials of said cosmetics comprise, in weight percentages:
11. the use of claim 10, wherein the emulsifier is at least one of stearic acid, steareth-21, and sodium stearoyl glutamate; the composite lipid material is at least one of glycerol tri (ethyl hexanoate), polydimethylsiloxane, stearyl alcohol, squalane, oleate and butanediol; the pH regulator is sodium hydroxide or citric acid; the water phase material is at least one of glycerol, sodium hyaluronate, glycosyl trehalose and carbomer; the preservative is at least one of methyl hydroxybenzoate, propyl hydroxybenzoate and phenoxyethanol.
12. The use according to claim 10, wherein the cosmetic is prepared by a process comprising: preparing stearyl glutamate sodium, sodium hydroxide, citric acid glycerol, sodium hyaluronate, glycosyl trehalose and carbomer into a water phase system, preparing stearic acid, steareth-21, glycerol tri (ethyl hexanoate) ester, polydimethylsiloxane, stearyl alcohol, squalane, oleate, butanediol, methyl hydroxybenzoate, propyl hydroxybenzoate and phenoxyethanol into an oil phase system, and respectively heating to 70-80 ℃; slowly adding the water phase system into the oil phase system, homogenizing at 80-95 deg.C until the paste turns into milk white, stirring for 3-5min, stopping heating, stirring at 40 deg.C, adding the microcapsule, stirring, and cooling to room temperature.
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| CN115024989A (en) * | 2022-06-01 | 2022-09-09 | 浙江迪恩生物科技股份有限公司 | Liposome prepared by coating curcumin or tetrahydrocurcumin with molecular motor vesicle and preparation method and application thereof |
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