CN106890102A - A kind of preparation method of Ascorbyl Tetraisopalmitate nano particle - Google Patents
A kind of preparation method of Ascorbyl Tetraisopalmitate nano particle Download PDFInfo
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- A—HUMAN NECESSITIES
- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/67—Vitamins
- A61K8/676—Ascorbic acid, i.e. vitamin C
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0241—Containing particulates characterized by their shape and/or structure
- A61K8/0279—Porous; Hollow
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
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- 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
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/413—Nanosized, i.e. having sizes below 100 nm
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- 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
- A61K2800/56—Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms
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Abstract
The present invention relates to a kind of preparation method of Ascorbyl Tetraisopalmitate nano particle, disperseed in including gellan gum, hydroxypropyl methyl cellulose, Sodium Hyaluronate are added into glycerine, butanediol, after be added thereto to water, open stirring and heat, cooling afterwards is added thereto to Ascorbyl Tetraisopalmitate, Phenoxyethanol, stir, obtain Ascorbyl Tetraisopalmitate sol solution；Sol solution is obtained into nano level sol solution by high-pressure homogeneous equipment afterwards；Sol solution is finally placed in freezen protective in liquid nitrogen.Ascorbyl Tetraisopalmitate nano particle prepared by this method, the excitant of Ascorbyl Tetraisopalmitate can be significantly reduced, product stability is greatly lifted, while its absorbability can be improved such that it is able to play more excellent anti-oxidant, whitening effect.
Description
Technical field
The present invention relates to a kind of preparation method of Ascorbyl Tetraisopalmitate nano particle, belong to cosmetic art neck
Domain.
Background technology
Vitamin C, also referred to as ascorbic acid, have many advantages when topical application, therefore widely should
For cosmetics and local pharmaceutical formulation.
Vitamin C has anti-oxidant, Bearberry Extract as cosmetic composition.Vitamin C as procollagen in corium it
Co-factor from amino acid and the hydroxylation of proline residue is improved skin elasticity, is reduced with the synthesis of stimulation collagen
Microgroove and wrinkle, vitamin C are exposed to produced by the skin of ultraviolet radiation certainly as effective antioxidant for removing
The injury induced by ultraviolet by base and protecting the skin from, vitamin C also supplementary function in other anti-oxidant dimensions of skin
The vitamin E of raw element, when TD, suppresses the B16 cell of epidermal melanocytes to prevent pigementation.By
In these beneficial effects, vitamin C has very big potentiality as topical cosmetic and the composition of medical formulation, for treatment or pre-
Prevent about pigementation and the skin aging of wrinkle.
However, vitamin C is easily oxidized flavescence, therefore it is difficult to be used in cosmetics.Therefore, it has been developed that
Many more stable vitamin C derivatives, such as sodium ascorbyl phosphate, L-Ascorbic Acid L-O-Phosphate, vitamin C glucoside, dimension
Raw element C ethylethers, Ascorbyl Tetraisopalmitate etc., but due to the problem of stability difference, cause its inoxidizability not good, together
When cause great obstacle in the presence of certain excitant, the application to vitamin C in cosmetics.
The content of the invention
A kind of deficiency that application of the present invention for existing vitamin C derivatives in cosmetics is present, there is provided Vitamin C
The preparation method of sour four different palmitate nano particles.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：
A kind of preparation method of Ascorbyl Tetraisopalmitate nano particle, it is characterised in that comprise the following steps：
1) Ascorbyl Tetraisopalmitate sol solution is prepared
By gellan gum 0.1-0.5 weight portions, hydroxypropyl methyl cellulose 0.1-0.5 weight portions, Sodium Hyaluronate 0.1-1 weights
Amount part be added to glycerine 1-5 weight portions, butanediol 1-5 weight portions in disperseed, after be added thereto to water 20-50 weight portions,
Open stirring and heat, be heated to 60-90 DEG C, be incubated 5-30min, after be cooled to 50 DEG C, after be added thereto to ascorbic acid four
Different palmitate 1-10 weight portions, Phenoxyethanol 0.5-0.8 weight portions, stir, and obtain Ascorbyl Tetraisopalmitate glue
Solution；
2) nanometer sol solution is prepared
By step 1) in gained sol solution by high-pressure homogeneous equipment, material is with the flow velocity spray of 1000~1500 meter per seconds
Go out, by the void effect, knock-on effect, the shearing effect that produce, obtain uniform, fine and smooth, nano level sol solution；
3) porous nano particle is prepared
By step 2) in the sol solution that obtains be placed in liquid nitrogen and freeze, in refrigerator is transferred to after product fully charge in-
Preserved in less than 18 DEG C of environment.
Further, step 2) described in high-pressure homogeneous equipment feed pressure control in 0.25-0.55MPa, homogenization pressure
It is 100-250MPa.
Further, step 1) described in mixing speed be 50-200r/min.
The beneficial effects of the invention are as follows：
This method is wrapped up and refined by the different palmitate of high pressure freezing Ascorbic Acid four, and what is obtained is anti-bad
The different palmitate nano particle of hematic acid four can significantly reduce the excitant of Ascorbyl Tetraisopalmitate, and greatly lifting is produced
Product stability, and then its inoxidizability can be improved such that it is able to play more excellent anti-oxidant, whitening effect.
Specific embodiment
Principle of the invention and feature are described below in conjunction with example, example is served only for explaining the present invention, and
It is non-for limiting the scope of the present invention.
Embodiment 1：
A kind of preparation method of Ascorbyl Tetraisopalmitate nano particle, comprises the following steps：
1) Ascorbyl Tetraisopalmitate sol solution is prepared
The weight portion of gellan gum 0.1, the weight portion of hydroxypropyl methyl cellulose 0.1, the weight portion of Sodium Hyaluronate 0.1 are added to
Disperseed in the weight portion of glycerine 1, the weight portion of butanediol 1, after be added thereto to the weight portion of water 20, open stirring and heat, plus
Heat to 70 DEG C, be incubated 20min, after be cooled to 50 DEG C, after be added thereto to the weight portion of Ascorbyl Tetraisopalmitate 1, benzene oxygen
The weight portion of ethanol 0.5, stirs, and obtains Ascorbyl Tetraisopalmitate sol solution；
2) nanometer sol solution is prepared
By step 1) in gained sol solution by high pressure homogenizer, feed pressure is controlled in 0.25-0.35MPa, homogeneous
Pressure is 100-120MPa, and material is sprayed with the flow velocity of 1000~1200 meter per seconds, by the void effect that produces, knock-on effect,
Shearing effect, obtains uniform, fine and smooth, nano level sol solution；
3) porous nano particle is prepared
By step 2) in the sol solution that obtains be placed in liquid nitrogen and freeze, in refrigerator is transferred to after product fully charge in-
Preserved in less than 18 DEG C of environment.
Embodiment 2：
A kind of preparation method of Ascorbyl Tetraisopalmitate nano particle, comprises the following steps：
1) Ascorbyl Tetraisopalmitate sol solution is prepared
The weight portion of gellan gum 0.4, the weight portion of hydroxypropyl methyl cellulose 0.2, the weight portion of Sodium Hyaluronate 0.2 are added to
Disperseed in the weight portion of glycerine 5, the weight portion of butanediol 1, after be added thereto to the weight portion of water 35, open stirring and heat, plus
Heat to 60 DEG C, be incubated 30min, after be cooled to 50 DEG C, after be added thereto to the weight portion of Ascorbyl Tetraisopalmitate 6, benzene oxygen
The weight portion of ethanol 0.8, stirs, and obtains Ascorbyl Tetraisopalmitate sol solution；
2) nanometer sol solution is prepared
By step 1) in gained sol solution by high-pressure homogeneous equipment, feed pressure is controlled in 0.35-0.45MPa,
Matter pressure is 120-130MPa, and material is sprayed with the flow velocity of 1200~1300 meter per seconds, by the void effect, the shock effect that produce
Should, shearing effect, obtain uniform, fine and smooth, nano level sol solution；
3) porous nano particle is prepared
By step 2) in the sol solution that obtains be placed in liquid nitrogen and freeze, in refrigerator is transferred to after product fully charge in-
Preserved in less than 18 DEG C of environment.
Embodiment 3：
A kind of preparation method of Ascorbyl Tetraisopalmitate nano particle, comprises the following steps：
1) Ascorbyl Tetraisopalmitate sol solution is prepared
The weight portion of gellan gum 0.5, the weight portion of hydroxypropyl methyl cellulose 0.5, the weight portion of Sodium Hyaluronate 1 are added to sweet
Disperseed in oily 5 weight portions, the weight portion of butanediol 5, after be added thereto to the weight portion of water 50, open stirring and heat, heating
To 60 DEG C, be incubated 30min, after be cooled to 50 DEG C, after be added thereto to the weight portion of Ascorbyl Tetraisopalmitate 10, benzene oxygen second
The weight portion of alcohol 0.8, stirs, and obtains Ascorbyl Tetraisopalmitate sol solution；
2) nanometer sol solution is prepared
By step 1) in gained sol solution by high-pressure homogeneous equipment, feed pressure is controlled in 0.45-0.55MPa,
Matter pressure is 180-200MPa, and material is sprayed with the flow velocity of 1300~1500 meter per seconds, by the void effect, the shock effect that produce
Should, shearing effect, obtain uniform, fine and smooth, nano level sol solution；
3) porous nano particle is prepared
By step 2) in the sol solution that obtains be placed in liquid nitrogen and freeze, in refrigerator is transferred to after product fully charge in-
Preserved in less than 18 DEG C of environment.
Embodiment 4：
A kind of preparation method of Ascorbyl Tetraisopalmitate nano particle, comprises the following steps：
1) Ascorbyl Tetraisopalmitate sol solution is prepared
The weight portion of gellan gum 0.1, the weight portion of hydroxypropyl methyl cellulose 0.1, the weight portion of Sodium Hyaluronate 0.1 are added to
Disperseed in the weight portion of glycerine 5, the weight portion of butanediol 5, after be added thereto to the weight portion of water 35, open stirring and heat, plus
Heat to 90 DEG C, be incubated 5min, after be cooled to 50 DEG C, after be added thereto to the weight portion of Ascorbyl Tetraisopalmitate 10, benzene oxygen
The weight portion of ethanol 0.5, stirs, and obtains Ascorbyl Tetraisopalmitate sol solution；
2) nanometer sol solution is prepared
By step 1) in gained sol solution by high pressure homogenizer, feed pressure is controlled in 0.25-0.35MPa, homogeneous
Pressure 220-250MPa, material is sprayed with the flow velocity of 1400~1500 meter per seconds, by the void effect of generation, knock-on effect, is cut
Effect is cut, uniform, fine and smooth, nano level sol solution is obtained；
3) porous nano particle is prepared
By step 2) in the sol solution that obtains be placed in liquid nitrogen and freeze, in refrigerator is transferred to after product fully charge in-
Preserved in less than 18 DEG C of environment.
Embodiment 5：
A kind of preparation method of Ascorbyl Tetraisopalmitate nano particle, comprises the following steps：
1) Ascorbyl Tetraisopalmitate sol solution is prepared
The weight portion of gellan gum 0.5, the weight portion of hydroxypropyl methyl cellulose 0.5, the weight portion of Sodium Hyaluronate 1 are added to sweet
Disperseed in oily 1 weight portion, the weight portion of butanediol 1, after be added thereto to the weight portion of water 20, open stirring and heat, heating
To 75 DEG C, be incubated 15min, after be cooled to 50 DEG C, after be added thereto to the weight portion of Ascorbyl Tetraisopalmitate 1, benzene oxygen second
The weight portion of alcohol 0.8, stirs, and obtains Ascorbyl Tetraisopalmitate sol solution；
2) nanometer sol solution is prepared
By step 1) in gained sol solution by high pressure homogenizer, feed pressure is controlled in 0.45-0.55MPa, homogeneous
Pressure is 120-130MPa, and material is sprayed with the flow velocity of 1200~1500 meter per seconds, by the void effect that produces, knock-on effect,
Shearing effect, obtains uniform, fine and smooth, nano level sol solution；
3) porous nano particle is prepared
By step 2) in the sol solution that obtains be placed in liquid nitrogen and freeze, in refrigerator is transferred to after product fully charge in-
Preserved in less than 18 DEG C of environment.
Embodiment 6：
A kind of preparation method of Ascorbyl Tetraisopalmitate nano particle, comprises the following steps：
1) Ascorbyl Tetraisopalmitate sol solution is prepared
The weight portion of gellan gum 0.4, the weight portion of hydroxypropyl methyl cellulose 0.2, the weight portion of Sodium Hyaluronate 0.2 are added to
Disperseed in the weight portion of glycerine 5, the weight portion of butanediol 5, after be added thereto to the weight portion of water 50, open stirring and heat, plus
Heat to 90 DEG C, be incubated 5min, after be cooled to 50 DEG C, after be added thereto to the weight portion of Ascorbyl Tetraisopalmitate 1, benzene oxygen second
The weight portion of alcohol 0.8, stirs, and obtains Ascorbyl Tetraisopalmitate sol solution；
2) nanometer sol solution is prepared
By step 1) in gained sol solution by high-pressure homogeneous equipment, feed pressure is controlled in 0.35-0.45MPa,
Matter pressure is 180-200MPa, and material is sprayed with the flow velocity of 1200~1500 meter per seconds, by the void effect, the shock effect that produce
Should, shearing effect, obtain uniform, fine and smooth, nano level sol solution；
3) porous nano particle is prepared
By step 2) in the sol solution that obtains be placed in liquid nitrogen and freeze, in refrigerator is transferred to after product fully charge in-
Preserved in less than 18 DEG C of environment.
Embodiment 7：
A kind of preparation method of Ascorbyl Tetraisopalmitate nano particle, comprises the following steps：
1) Ascorbyl Tetraisopalmitate sol solution is prepared
The weight portion of gellan gum 0.1, the weight portion of hydroxypropyl methyl cellulose 0.1, the weight portion of Sodium Hyaluronate 0.1 are added to
Disperseed in the weight portion of glycerine 5, the weight portion of butanediol 1, after be added thereto to the weight portion of water 50, open stirring and heat, plus
Heat to 90 DEG C, be incubated 5min, after be cooled to 50 DEG C, after be added thereto to the weight portion of Ascorbyl Tetraisopalmitate 10, benzene oxygen
The weight portion of ethanol 0.5, stirs, and obtains Ascorbyl Tetraisopalmitate sol solution；
2) nanometer sol solution is prepared
By step 1) in gained sol solution by high-pressure homogeneous equipment, feed pressure is controlled in 0.25-0.35MPa,
Matter pressure is 100-120MPa, and material is sprayed with the flow velocity of 1200~1500 meter per seconds, by the void effect, the shock effect that produce
Should, shearing effect, obtain uniform, fine and smooth, nano level sol solution；
3) porous nano particle is prepared
By step 2) in the sol solution that obtains be placed in liquid nitrogen and freeze, in refrigerator is transferred to after product fully charge in-
Preserved in less than 18 DEG C of environment.
Embodiment 8：
A kind of preparation method of Ascorbyl Tetraisopalmitate nano particle, comprises the following steps：
1) Ascorbyl Tetraisopalmitate sol solution is prepared
The weight portion of gellan gum 0.3, the weight portion of hydroxypropyl methyl cellulose 0.3, the weight portion of Sodium Hyaluronate 0.2 are added to
Disperseed in the weight portion of glycerine 1, the weight portion of butanediol 1, after be added thereto to the weight portion of water 20, open stirring and heat, plus
Heat to 60 DEG C, be incubated 30min, after be cooled to 50 DEG C, after be added thereto to the weight portion of Ascorbyl Tetraisopalmitate 6, benzene oxygen
The weight portion of ethanol 0.8, stirs, and obtains Ascorbyl Tetraisopalmitate sol solution；
2) nanometer sol solution is prepared
By step 1) in gained sol solution by high-pressure homogeneous equipment, feed pressure is controlled in 0.35-0.45MPa,
Matter pressure is 180-200MPa, and material is sprayed with the flow velocity of 1200~1500 meter per seconds, by the void effect, the shock effect that produce
Should, shearing effect, obtain uniform, fine and smooth, nano level sol solution；
3) porous nano particle is prepared
By step 2) in the sol solution that obtains be placed in liquid nitrogen and freeze, in refrigerator is transferred to after product fully charge in-
Preserved in less than 18 DEG C of environment.
In order to verify the technique effect of the nano particle that preparation method of the invention is obtained, We conducted following test：
First, security test
1.1 test materials
Spot tries device：The production of Beijing North doctor's management of investment Co., Ltd, circular, diameter 12mm.
Spot tries thing：The ascorbic acid four of the Ascorbyl Tetraisopalmitate solution of 5wt%, the gained of embodiment 2 of 5wt%
Different palmitate nano-solid solution.
1.2 Subject Populations and testing time
Effective subject amounts to 30 people, and specific sex composition and age composition determine (to meet 2007 at random《Cosmetics health
Specification》Include, exclusion standard.
1.3 experimental techniques
Subject is selected by subject enrollment standard, number is 30.From qualified patch material, sample is put into spot
In examination device (amount of samples is 0.020g-0.025g), control wells are blank (not putting any material).Sample and blank is equal
The forearm song side of subject is affixed on, is gently pressed with palm and is allowed to equably be pasted on skin, continue 24h.Between after removal patch device
Every 30min, dermoreaction is observed after impression disappears.24h and 48h are observed once again respectively after patch test, and observation skin is anti-
Should.Skin adverse reaction grade scale is shown in Table 1：
Table 1：Skin adverse reaction is classified
1.4 results are explained：
Skin closure type patch test results are explained：Occur 1 grade of number of skin adverse reaction in 30 subjects and be more than 5
Example, or 2 grades of numbers of skin adverse reaction are more than 2, or when there is any 13 grades or more than 3 grades skin adverse reactions, sentence
Determine tested material has adverse reaction to human body.
1.5 experimental results
Result of the test is shown in Table 2,3,4.
The removal spot examination 0.5 hour observation result of device of table 2
The removal spot examination 24 hours observation results of device of table 3
The removal spot examination 48 hours observation results of device of table 4
Test result indicate that：This patch test results, according to 2007《Cosmetics health specification》Requirement, judge
The Ascorbyl Tetraisopalmitate solution of 5wt% has adverse reaction, the different palmitic acid of ascorbic acid four of 5wt% to human body skin
Ester nano-solid solution has no adverse reaction to human body.
2nd, stability test
2.1. heat-resistant stability investigates experiment
Experimental technique be by the 10wt% Ascorbyl Tetraisopalmitate nano-solid solution of the gained of embodiment 3 with
Each 100 grams of 10wt% Ascorbyl Tetraisopalmitate solution, is put into 100 grams of transparent plastic bottles (pharmaceutical grade), sealing, is put into
In 60 degree of baking ovens, observation changes over time the discoloration of sample, judges the Heat-resistant stable sex differernce of the two, and concrete outcome is shown in Table
5。
The heat-resistant stability of table 5 investigates experiment
Test result indicate that：10wt% Ascorbyl Tetraisopalmitates solution occurred turning yellow when heat-resisting 5th day
Phenomenon, and as the lengthening color of heat-resistant time is gradually deepened, stability is gradually deteriorated with time lengthening, 10wt% ascorbic acid
Four different palmitate nano-solid solution are faint yellow in appearance in the 15th day, and the time is more molten than 10wt% Ascorbyl Tetraisopalmitate
In 10 days evenings of liquid, the active matter prepared through high pressure freezing is illustrated, heat-resistant stability is increased dramatically.
2.2 light durabilities investigate experiment
Experimental technique is by 10wt% Ascorbyl Tetraisopalmitate nano-solid solution and 10wt% ascorbic acid four
Each 100 grams of different palmitate solution, is put into 100 grams of transparent plastic bottles (pharmaceutical grade), sealing, is put into the experiment under sunlight irradiation
On platform, observation changes over time the discoloration of sample, judges the Heat-resistant stable sex differernce of the two, and concrete outcome is shown in Table 6.
The light shine study on the stability of table 6 is tested
Test result indicate that：10wt% Ascorbyl Tetraisopalmitates solution occurred turning yellow when heat-resisting 5th day
Phenomenon, and as the lengthening color of heat-resistant time is gradually deepened, stability is gradually deteriorated with time lengthening, 10wt% ascorbic acid
Four different palmitate nano-solid solution are faint yellow in appearance in the 20th day, and the time is more molten than 10wt% Ascorbyl Tetraisopalmitate
In 15 days evenings of liquid, the active matter prepared through high pressure freezing is illustrated, heat-resistant stability is increased dramatically.
3rd, it is both effectiveness
3.1 inoxidizability
Experiment carries out the measure to DPPH free radical scavenging activities to the sample before and after parcel, is divided to two groups to carry out contrast test,
One group is Ascorbyl Tetraisopalmitate (0.1%, 0.2%, 0.3%, 0.4%, 0.5%) five kinds of different quality concentration, one
Group is the Ascorbyl Tetraisopalmitate nano-solid (0.1%, 0.2%, 0.3%, 0.4%, 0.5%) of the gained of embodiment 4
Five kinds of different quality concentration.
Specific experiment step takes 2mL, plus 2mL × 10 to take every kind of sample-4Mol/L DPPH are mixed, and are kept away under room temperature condition
Light reaction 20min, 4000r/min centrifugation 10min, takes supernatant mensuration absorbance Ai at 517nm wavelength.Blank group is with grade body
95% ethanol solution of product replaces DPPH solution, and control group replaces sample solution with isometric deionized water, by the ethanol of 2mL 95%
It is mixed for zeroing with isometric deionized water.According to formula determination sample clearance rate.Computing formula is SA (%)=1- (Ai-
Aj)/A0 × 100%
A0:The absorbance of DPPH and solvent mixed liquor
Ai:Absorbance after DPPH and example reaction
Aj:The absorbance of sample and solvent mixed liquor
Specific test result is shown in Table 7
The scavenging action of table 7DPPH free radicals is compared
Test result indicate that：The ascorbic acid palm fibre under the addition concentration of (0.1%, 0.2%, 0.3%, 0.4%, 0.5%)
Glycerin monostearate nano-solid is significantly increased compared with the antioxygenic property of Ascorbyl Tetraisopalmitate, illustrates through high pressure freezing
The active matter of preparation, antioxygenic property is increased dramatically.
3.2 whitening performances
3.2.1 instrument：Spectrophotometer, micropipettor (1mL), electronic balance, volumetric flask (10mL, 50mL,
250mL), constant temperature water box, beaker and graduated cylinder are some.
3.2.2 sample：Potato, TYR, sodium dihydrogen phosphate, disodium hydrogen phosphate, deionized water
3.2.3 preparation of reagents：
PBS (pH=6.8)：The sodium dihydrogen phosphate of 0.2mol/L and the phosphorus of 0.2mol/L are first prepared respectively
Sour disodium hydrogen.
0.2mol/L sodium dihydrogen phosphates：Weigh 71.6g Na2HPO4-12H2O, is dissolved in 1000mL deionized waters；
0.2mol/L disodium hydrogen phosphates：Weigh 31.2g NaH2PO4-2H2O, is dissolved in 1000mL deionized waters；
Take the phosphate buffer that 51mL sodium dihydrogen phosphate+49mL disodium hydrogen phosphates obtain final product 0.2mol/L, pH=6.8.
TYR solution：TYR 25.6g is weighed, with phosphate buffer constant volume in 50mL volumetric flasks, L- is obtained final product
Tyrosine solution.
Tyrosinase solution：Potato is cleaned, in 4 DEG C of precooling 4h or so.Peeling, is cut into about 1.0cm3Fourth shape, in -20
DEG C freeze overnight.Weigh, by 1：1(W:V ratio) adds 4 DEG C of sodium phosphate buffers of precooling, is made of tissue mashing machine even
Slurry, 3 layers of filtered through gauze, filtrate is centrifuged 10min in 4000r/min, and supernatant is the tyrosinase crude enzyme liquid of gained, 4 DEG C of guarantors
Deposit, be finished in 2h.
Ascorbyl Tetraisopalmitate is prepared by test solution：Ascorbyl Tetraisopalmitate is made into 5mg/mL's
Solution and with methanol dilution to 1mg/mL.
Ascorbyl Tetraisopalmitate nano-solid is prepared by test solution：Ascorbyl Tetraisopalmitate nanometer is solid
Body is made into the solution of 5mg/mL and with methanol dilution to 1mg/mL.
3.2.4 experimental technique
According to table 8 Suo Shi to phosphate buffer, sample solution, tyrosine solution is sequentially added in test tube, in 35 DEG C of water
Bath 10 minutes.Tyrosine enzyme liquid is subsequently adding, is mixed, then 30min is incubated at 35 DEG C, be transferred quickly in cuvette,
Mensuration absorbance at 475nm.
The composition of the prepare liquid of table 8
| Sample | A groups | B groups | C groups | D groups |
| 1mg/mL sample solutions | 1mL | 1mL | ||
| PH6.8 phosphate buffers | 1mL | 1mL | 1mL | 1mL |
| 0.15%L- tyrosine solutions | 1mL | 1mL | ||
| Tyrosinase solution | 1mL | 1mL |
Using each group absorbance, by calculating tyrosinase inhibition rate, its computing formula is as follows:
A:It is not loaded the absorbance A (a) that the enzyme-added mixed liquor of product is surveyed；
B:It is not loaded the absorbance A (b) that the also not enzyme-added mixed liquor of product is surveyed；
C:The absorbance A (c) that the mixed liquor of sample-adding product and enzyme is surveyed；
D:Sample-adding product and absorbance A (d) that not enzyme-added mixed liquor is surveyed.
3.2.5 experimental result
By above-mentioned detection method, 2 kinds are detected by test solution, draw the inhibiting rate of the two, be specifically shown in Table 9：
9 two kinds of inhibiting rates by test solution of table compare
Test result indicate that：Suppression of the Ascorbyl Tetraisopalmitate nano-solid compared with Ascorbyl Tetraisopalmitate
The ability of tyrosinase is significantly increased, and tyrosinase inhibition rate is higher, and the melanin generated in skin is fewer, whitening effect
Will be better, the active matter prepared through high pressure freezing is illustrated, whitening performance is increased dramatically.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all it is of the invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (3)
1. a kind of preparation method of Ascorbyl Tetraisopalmitate nano particle, it is characterised in that comprise the following steps：
1) Ascorbyl Tetraisopalmitate sol solution is prepared
By gellan gum 0.1-0.5 weight portions, hydroxypropyl methyl cellulose 0.1-0.5 weight portions, Sodium Hyaluronate 0.1-1 weight portions
Be added in glycerine 1-5 weight portions, butanediol 1-5 weight portions and disperseed, after be added thereto to water 20-50 weight portions, open
Stirring and heat, be heated to 60-90 DEG C, be incubated 5-30min, after be cooled to 50 DEG C, after be added thereto to the different palm fibre of ascorbic acid four
Glycerin monostearate 1-10 weight portions, Phenoxyethanol 0.5-0.8 weight portions, stir, and obtain Ascorbyl Tetraisopalmitate sol solution；
2) nanometer sol solution is prepared
By step 1) in gained sol solution by high-pressure homogeneous equipment, material is sprayed with the flow velocity of 1000~1500 meter per seconds, logical
Void effect, knock-on effect, the shearing effect for producing are crossed, uniform, fine and smooth, nano level sol solution is obtained；
3) porous nano particle is prepared
By step 2) in the sol solution that obtains be placed in liquid nitrogen and freeze, in -18 DEG C in refrigerator is transferred to after product fully charge
Preserved in following environment.
2. preparation method according to claim 1, it is characterised in that step 2) described in high-pressure homogeneous equipment charging pressure
Power is controlled in 0.25-0.55MPa, and homogenization pressure is 100-250MPa.
3. preparation method according to claim 1 and 2, it is characterised in that step 1) described in mixing speed be 50-
200r/min。
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| CN101214199A (en) * | 2007-12-29 | 2008-07-09 | 广东拉芳日化有限公司 | Nano active acne-eliminating cosmetic composition |
| CN104857567A (en) * | 2015-05-11 | 2015-08-26 | 华南理工大学 | Calcium alginate/hydroxyapatite nano compound double drug loading porous scaffold containing biodegradable polyester microspheres and preparation method thereof |
| CN106214511A (en) * | 2016-08-22 | 2016-12-14 | 上海乐宝日化股份有限公司 | A kind of whitening lotion containing liposome and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101214199A (en) * | 2007-12-29 | 2008-07-09 | 广东拉芳日化有限公司 | Nano active acne-eliminating cosmetic composition |
| CN104857567A (en) * | 2015-05-11 | 2015-08-26 | 华南理工大学 | Calcium alginate/hydroxyapatite nano compound double drug loading porous scaffold containing biodegradable polyester microspheres and preparation method thereof |
| CN106214511A (en) * | 2016-08-22 | 2016-12-14 | 上海乐宝日化股份有限公司 | A kind of whitening lotion containing liposome and preparation method thereof |
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