CN108524312B - A kind of sulforaphen pik woods micro emulsion and preparation method thereof - Google Patents
A kind of sulforaphen pik woods micro emulsion and preparation method thereof Download PDFInfo
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- 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
- A61K8/46—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
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- A61K8/068—Microemulsions
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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
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- A61K8/645—Proteins of vegetable origin; Derivatives or degradation products thereof
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- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of 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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- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
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Abstract
The present invention relates to a kind of sulforaphen pik woods micro emulsions and preparation method thereof, it is characterized in that, including following components: 1.2~2.5% zeins, 0.3~0.6% corn glycogen, 0.02~0.12% sodium chloride, 5.0~15.0% ethyl alcohol, 12.0~25.0% ring five dimethyl silicone polymer, 4.8~13.5% methyl pyrrolidone, 3.0~5.0% sulforaphen, 3.0~8.0% isononyl isononanoate, 2.0~5.0% vegetable oil, 0.50% Phenoxyethanol, surplus is distilled water, and the percentage is mass percent.The resulting sulforaphen pik woods micro emulsion of the present invention is with irritation is small, Transdermal absorption is good, drugloading rate is big, skin sense is good, the simple advantage of preparation process.
Description
Technical field
The present invention relates to pik woods (Pickering) micro emulsion preparation technical field, in particular to a kind of sulforaphen pik
Woods micro emulsion and preparation method thereof.
Background technique
Sulforaphen (Sulforaphane, Sulforaphane), also known as " sulforaphane ", mainly
It is present in the crucifers such as radish, Chinese cabbage, broccoli, there is good anticancer effect, applied in cosmetic industry
With antipollution and anti-oxidation efficacy.Sulforaphen activity is strong, vulnerable to the influence of environment temperature, illumination and pH value, at normal temperature
It easily decomposes, changes colour, is spoiled.The research of the raising sulforaphen stability occurred in presently relevant document, such as patent
A kind of preparation method of sulforaphen micro emulsion rapid-released droppills, patent are reported in CN201710077085.7
CN201210023702.2 reports a kind of microcapsule embedded method etc. of sulforaphen, but be mostly be directed to pharmaceuticals industry into
Capable exploitation.In cosmetic industry, there is presently no the effective methods of report to stablize sulforaphen, thus limits it and answer
With.
Pik woods micro emulsion is a kind of to stablize two kinds of immiscible liquid as emulsifier by nano-scale solid particle
And the microemulsion prepared, the emulsification of conventional emulsifier is replaced using solid particle, save the cost, irritation are low.Traditional skin
Solid particle used in crin lotion mainly has diatomite, montmorillonite and nanometer polymerization composition granule etc., tight between solid particle
It is close to be arranged together, play the role of steric hindrance, so that the aggregation between inhibiting dispersant liquid drop, enhances emulsion intercalation method.
But diatomite, montmorillonite and nanometer polymerization composition granule are that hardness is higher, the very puckery solid powder of feel, using in cosmetics
The use feeling of product can be deteriorated.
Zeins (Zein) is the natural macromolecular material extracted from corn protein powder, average molecular weight 25~
45kDa, average grain diameter 100-350nm include hydrophobic residue and some polar groups in molecule, are one kind typical two
Parent's property polymer is well suited as the Pickering agent of pickering emulsion；Corn glycogen (Glycogen) is one kind by glucose
Dendritic branch polysaccharide made of condensation, is directly extracted from corn, and average molecular weight is 1500~2500kDa, average grain diameter
For 30-80nm, have amphipathic, pickering emulsion can be stablized；And the sense of both the above solid powder skin is soft fine and smooth, use feeling
Well.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of sulforaphen pik woods micro emulsion and preparation method thereof, gained trailing plants
Thionin pik woods micro emulsion is foretold with irritation is small, Transdermal absorption is good, drugloading rate is big, skin sense is good, the simple advantage of preparation process.
In order to solve the above technical problems, the invention adopts the following technical scheme: a kind of sulforaphen pik woods micro emulsion, special
Sign is, including following components: 1.2~2.5% zeins, 0.3~0.6% corn glycogen, 0.02~0.12%
Sodium chloride, 5.0~15.0% ethyl alcohol, 12.0~25.0% ring five dimethyl silicone polymer, 4.8~13.5% methylpyrrole
Alkanone, 3.0~5.0% sulforaphen, 3.0~8.0% isononyl isononanoate, 2.0~5.0% vegetable oil, 0.50% benzene
Oxyethanol, surplus are distilled water, and the percentage is mass percent.
A kind of preparation method of sulforaphen pik woods micro emulsion, it is characterised in that use following steps:
A, weigh raw material according to following mass ratio: 1.2~2.5% zeins, 0.3~0.6% corn glycogen,
0.02~0.12% sodium chloride, 5.0~15.0% ethyl alcohol, 12.0~25.0% ring five dimethyl silicone polymers, 4.8~13.5% methyl
Pyrrolidones, 3.0~5.0% sulforaphens, 3.0~8.0% isononyl isononanoates, 2.0~5.0% vegetable oil, 0.50% benzene oxygen second
Alcohol, surplus are distilled water；The vegetable oil is avocado oil, linseed oil, white pond flower seed oil, hippophae rhamnoides fruit oil, camellia seed oil, wheat
One of embryo oil, samara oil, jojoba oil or their mixture；
B, by the zeins and ethyl alcohol, put into emulsion pot, at room temperature with 100~200rpm speed stir to
It is completely dissolved, then puts into the distilled water, corn glycogen, stirred to being completely dissolved, most with 300~450rpm speed at room temperature
After the sodium chloride, Phenoxyethanol is added, obtain aqueous dispersion liquid, citric acid-sodium citrate buffer be added by the water
The pH value of phase dispersant liquid is adjusted to 6.0~7.0；
C, the sulforaphen and methyl pyrrolidone are added to oily phase pot, the ring five poly- two is added after being dispersed with stirring
Methylsiloxane, isononyl isononanoate, vegetable oil obtain miscella phase；
D, gained miscella phase in step C is mixed in emulsion pot with step B gained aqueous dispersion liquid, with 500~
The revolving speed of 650rpm stirs 30min, obtains sulforaphen pik woods premixed solution；
E, gained sulforaphen pik woods premixed solution in step D is put into high pressure homogenizer, at room temperature in 1000bar
Homogeneous 5~10 times under (100MPa) pressure, each 3~8min of homogeneous obtain sulforaphen pik woods microemulsion.
After tested, sulforaphen pik woods microemulsion prepared by the present invention is O/W type, and pH value range is 5.80~6.80,
Rotary viscosity range 1000~4000cps(Brookfield viscosimeter, 2# rotor, revolving speed 6RPM), the drugloading rate of sulforaphen
2.82~4.50wt%, Malvern particle size analyzer measure the average-size of oil droplet between 60~90nm, are uniformly dispersed, and fluorescence is aobvious
Micro mirror studies absorption situation of the particle at oil-water interfaces, observes visible present invention gained sulforaphen pik woods microemulsion oil
Drop surface has coated fine and close nanoparticle membrana granulosa, and without aggregation between oil droplet, is centrifuged stable testing through 5000rpm, 30min
It is not stratified, 50 DEG C, save under -10 DEG C of environment three months it is not stratified, non-discolouring.
The sulforaphen pik woods microemulsion prepared in the present invention, collocation use the zeins of relatively small molecular weight
The corn glycogen (average molecular weight 1500kDa) of (average molecular weight 30kDa) and macromolecule is used as pik woods compound emulsifying agent,
To fill the gap between different molecular weight emulsifier, close adsorption layer can be formed in oil droplets, interfacial film is not easily broken, surely
It is qualitative fabulous.
The sulforaphen pik woods microemulsion prepared in the present invention, the drugloading rate of sulforaphen are up to 2.82~4.50wt%,
This is because steric hindrance caused by corn glycogen high score branch structure can reduce the mobility of bioactive molecule, dendritic structure is permitted
Perhaps bioactive molecule particle in its adsorption and keeps stablizing, therefore is greatly improved the drugloading rate of sulforaphen.
Using sulforaphen pik woods microemulsion prepared in the specific embodiment of the invention 1 as reference sample A, control examination is carried out
It tests, properties of samples parameter is listed in table 1.
Check experiment is 1.
A, raw material: 1.8% zeins, 0.08% sodium chloride, 10.0% ethyl alcohol, 20.0% is weighed according to following mass ratio
Ring five dimethyl silicone polymer, 8.0% methyl pyrrolidone, 4.0% sulforaphen, 8.0% isononyl isononanoate, 3.5% fructus hippophae
Oil, 0.50% Phenoxyethanol, surplus are distilled water；
B, by zeins and ethyl alcohol, emulsion pot is put into, is stirred with 200rpm speed to being completely dissolved, is connect at room temperature
The load weighted distilled water of investment, corn glycogen, stirred at room temperature with 300rpm speed to being completely dissolved, chlorination be then added
Sodium, Phenoxyethanol obtain aqueous dispersion liquid, and citric acid-sodium citrate buffer solution is added and is adjusted to the pH value of aqueous dispersion liquid
7.0；
C, sulforaphen and methyl pyrrolidone are added to oily phase pot, are dispersed with stirring in advance, ring five poly- two is then added
Methylsiloxane, isononyl isononanoate, hippophae rhamnoides fruit oil obtain miscella phase；
D, gained miscella phase in step C is mixed in emulsion pot with aqueous dispersion liquid obtained by step B, with 650rpm's
Revolving speed stirs 30min, obtains sulforaphen pik woods premixed solution；
E, gained sulforaphen pik woods premixed solution in step D is put into high pressure homogenizer, at room temperature in 1000bar
Homogeneous 8 times under (100MPa) pressure, each homogeneous 5min obtain sulforaphen pik woods microemulsion, are sample B.
Check experiment is 2.
A, raw material: 0.60% corn glycogen, 0.08% sodium chloride, 10.0% ethyl alcohol, 20.0% ring is weighed according to following mass ratio
Five dimethyl silicone polymers, 8.0% methyl pyrrolidone, 4.0% sulforaphen, 8.0% isononyl isononanoate, 3.5% hippophae rhamnoides fruit oil,
0.50% Phenoxyethanol, surplus are distilled water；
1. remaining step, obtains sulforaphen pik woods microemulsion with check experiment, be sample C.
1 properties of samples parameter of table
Sample A: compound emulsifying agent: zeins and corn glycogen；
Sample B: single emulsifier: zeins；
Sample C: single emulsifier: corn glycogen.
Through check experiment it is found that the present invention utilizes the zeins of nano-scale and primverose original work are compound pik
Woods emulsifier can significantly improve drugloading rate of the sulforaphen in pik woods microemulsion, and sulforaphen is greatly improved
Stability.
Gained sulforaphen pik woods microemulsion oil droplet average-size is Nano grade in the present invention, between 60~90nm,
It is uniformly dispersed, has many advantages, such as that partial size is small, is easy to permeate, transdermal absorption factor is high and bioavilability is high, can repair skin with deep layer
Skin is applied in cosmetic industry, has huge market value.
Viscosity is lower under gained sulforaphen pik woods microemulsion room temperature in the present invention, and good fluidity may be directly applied to
In cosmetic formulations exploitation, it is proposed that additive amount 2.0~5.0% can be added into directly below in O/W type skin care item formula in 40 DEG C
It stirs evenly, while bringing anti-inflammatory, anti-oxidation efficacy, provides silk abundant sliding soft skin sense.
In conclusion the present invention is pik woods emulsifier using compound zeins and primverose original work, in conjunction with height
Pressure homogeneous technology prepares sulforaphen pik woods microemulsion, has the advantages that 1, the use of emulsifier is greatly saved
It measures, not only save the cost, while being greatly reduced irritation；2, the pik woods micro emulsion oil droplet average grain diameter prepared is nanoscale,
Between 60~90nm, be conducive to the Transdermal absorption and infiltration of sulforaphen, achieve the purpose that deep layer repairs skin；3, sulforaphen
Drugloading rate is up to 2.82~4.50wt%, improves 10 times or so than traditional packaging method drugloading rate, and effectively improve radish sulphur
The storage stability and usability of element；4, product skin sense flexible silk is sliding, and the usability in cosmetics is high, and stability is good, guarantees the quality
Not stratified non-discolouring in phase, preparation process is simple and environmentally-friendly.
Specific embodiment
Present invention be described in more detail combined with specific embodiments below, but the present invention is not limited to these embodiments.
Embodiment 1:
A kind of preparation method of sulforaphen pik woods micro emulsion, it is characterised in that use following steps:
A, weigh raw material according to following mass ratio: 1.8% zeins, 0.6% corn glycogen, 0.08% sodium chloride,
10.0% ethyl alcohol, 20.0% ring five dimethyl silicone polymer, 8.0% methyl pyrrolidone, 4.0% sulforaphen, 8.0% isononanoic acid are different
Nonyl ester, 3.5% hippophae rhamnoides fruit oil, 0.50% Phenoxyethanol, surplus are distilled water；
B, by zeins and ethyl alcohol, emulsion pot is put into, is stirred at room temperature with 200rpm speed to being completely dissolved,
Then load weighted distilled water, corn glycogen are put into, is stirred at room temperature with 300rpm speed to being completely dissolved, is eventually adding chlorination
Sodium, Phenoxyethanol, obtain aqueous dispersion liquid, are adjusted to the pH value of aqueous dispersion liquid using citric acid-sodium citrate buffer solution
7.0；
C, sulforaphen and methyl pyrrolidone are added to oily phase pot, five polydimethylsiloxanes of ring is added after being dispersed with stirring
Alkane, isononyl isononanoate, hippophae rhamnoides fruit oil obtain miscella phase；
D, gained miscella phase in step C is mixed in emulsion pot with aqueous dispersion liquid obtained by step B, with 650rpm's
Revolving speed stirs 30min, obtains sulforaphen pik woods premixed solution；
E, gained sulforaphen pik woods premixed solution in step D is put into high pressure homogenizer, at room temperature in 1000bar
Homogeneous 8 times under (100MPa) pressure, each homogeneous 5min obtain sulforaphen pik woods microemulsion.
Sulforaphen pik woods microemulsion pH value 6.80 obtained by the present embodiment, rotary viscosity 2800cps(Brookfield are viscous
Degree meter, 2# rotor, revolving speed 6RPM), the average-size of sulforaphen drugloading rate 3.75wt%, oil droplet are 75nm, it is uniformly dispersed, oil
Without aggregation between drop, through 5000rpm, it is not stratified that 30min is centrifuged stable testing, 50 DEG C, save under -10 DEG C of environment three months regardless of
Layer, it is non-discolouring.
Embodiment 2:
A kind of preparation method of sulforaphen pik woods micro emulsion, it is characterised in that use following steps:
A, weigh raw material according to following mass ratio: 1.2% zeins, 0.3% corn glycogen, 0.02% sodium chloride,
5.0% ethyl alcohol, 12.0% ring five dimethyl silicone polymer, 10.5% methyl pyrrolidone, 3.0% sulforaphen, 6.0% isononanoic acid are different
Nonyl ester, 2.5% avocado oil, 2.5% white pond flower seed oil, 0.50% Phenoxyethanol, surplus are distilled water；
B, by zeins and ethyl alcohol, emulsion pot is put into, is stirred at room temperature with 100rpm speed to being completely dissolved,
Then load weighted distilled water, corn glycogen are put into, is stirred at room temperature with 450rpm speed to being completely dissolved, is eventually adding chlorination
Sodium, Phenoxyethanol, obtain aqueous dispersion liquid, are adjusted to the pH value of aqueous dispersion liquid using citric acid-sodium citrate buffer solution
6.0；
C, sulforaphen and methyl pyrrolidone are added to oily phase pot, five polydimethylsiloxanes of ring is added after being dispersed with stirring
Alkane, isononyl isononanoate, avocado oil, white pond flower seed oil, obtain miscella phase；
D, gained miscella phase in step C is mixed in emulsion pot with aqueous dispersion liquid obtained by step B, with 500rpm's
Revolving speed stirs 30min, obtains sulforaphen pik woods premixed solution；
E, gained sulforaphen pik woods premixed solution in step D is put into high pressure homogenizer, at room temperature in 1000bar
Homogeneous 10 times under (100MPa) pressure, each homogeneous 3min obtain sulforaphen pik woods microemulsion.
Sulforaphen Pickering microemulsion pH value 5.80, rotary viscosity 1000cps obtained by the present embodiment
(Brookfield viscosimeter, 2# rotor, revolving speed 6RPM), sulforaphen drugloading rate 2.82wt%, the average-size of oil droplet are
60nm is uniformly dispersed, and without aggregation between oil droplet, through 5000rpm, 30min centrifugation stable testing is not stratified, 50 DEG C, -10 DEG C of environment
Lower preservation three months not stratified, non-discolouring.
Embodiment 3:
A kind of preparation method of sulforaphen pik woods micro emulsion, it is characterised in that use following steps:
A, weigh raw material according to following mass ratio: 2.5% zeins, 0.5% corn glycogen, 0.12% sodium chloride,
15.0% ethyl alcohol, 25.0% ring five dimethyl silicone polymer, 12.5% methyl pyrrolidone, 5.0% sulforaphen, 3.0% isononanoic acid are different
Nonyl ester, 2.0% linseed oil, 0.50% Phenoxyethanol, surplus are distilled water；
B, by zeins and ethyl alcohol, emulsion pot is put into, is stirred at room temperature with 200rpm speed to being completely dissolved,
Then load weighted distilled water, corn glycogen are put into, is stirred at room temperature with 350rpm speed to being completely dissolved, is eventually adding chlorination
Sodium, Phenoxyethanol, obtain aqueous dispersion liquid, are adjusted to the pH value of aqueous dispersion liquid using citric acid-sodium citrate buffer solution
6.5；
C, sulforaphen and methyl pyrrolidone are added to oily phase pot, five polydimethylsiloxanes of ring is added after being dispersed with stirring
Alkane, isononyl isononanoate, linseed oil obtain miscella phase；
D, gained miscella phase in step C is mixed in emulsion pot with aqueous dispersion liquid obtained by step B, with 600rpm's
Revolving speed stirs 30min, obtains sulforaphen pik woods premixed solution；
E, gained sulforaphen pik woods premixed solution in step D is put into high pressure homogenizer, at room temperature in 1000bar
Homogeneous 6 times under (100MPa) pressure, each homogeneous 4min obtain sulforaphen pik woods microemulsion.
Sulforaphen Pickering microemulsion pH value 6.20, rotary viscosity 4000cps obtained by the present embodiment
(Brookfield viscosimeter, 2# rotor, revolving speed 6RPM), sulforaphen drugloading rate 4.50wt%, the average-size of oil droplet are
82nm is uniformly dispersed, and without aggregation between oil droplet, through 5000rpm, 30min centrifugation stable testing is not stratified, 50 DEG C, -10 DEG C of environment
Lower preservation three months not stratified, non-discolouring.
Embodiment 4:
A kind of preparation method of sulforaphen pik woods micro emulsion, it is characterised in that use following steps:
A, weigh raw material according to following mass ratio: 1.5% zeins, 0.4% corn glycogen, 0.06% sodium chloride,
8.0% ethyl alcohol, 22.0% ring five dimethyl silicone polymer, 4.8% methyl pyrrolidone, 3.2% sulforaphen, the different nonyl of 7.0% isononanoic acid
Ester, 2.0% camellia seed oil, 2.0% wheat-germ oil, 0.50% Phenoxyethanol, surplus are distilled water；
B, by zeins and ethyl alcohol, emulsion pot is put into, is stirred at room temperature with 120rpm speed to being completely dissolved,
Then load weighted distilled water, corn glycogen are put into, is stirred at room temperature with 320rpm speed to being completely dissolved, is eventually adding chlorination
Sodium, Phenoxyethanol, obtain aqueous dispersion liquid, are adjusted to the pH value of aqueous dispersion liquid using citric acid-sodium citrate buffer solution
6.3；
C, sulforaphen and methyl pyrrolidone are added to oily phase pot, five polydimethylsiloxanes of ring is added after being dispersed with stirring
Alkane, isononyl isononanoate, camellia seed oil, wheat-germ oil obtain miscella phase；
D, gained miscella phase in step C is mixed in emulsion pot with aqueous dispersion liquid obtained by step B, with 550rpm's
Revolving speed stirs 30min, obtains sulforaphen pik woods premixed solution；
E, gained sulforaphen pik woods premixed solution in step D is put into high pressure homogenizer, at room temperature in 1000bar
Homogeneous 5 times under (100MPa) pressure, each homogeneous 8min obtain sulforaphen pik woods microemulsion.
Sulforaphen Pickering microemulsion pH value 5.95, rotary viscosity 2200cps obtained by the present embodiment
(Brookfield viscosimeter, 2# rotor, revolving speed 6RPM), sulforaphen drugloading rate 3.05wt%, the average-size of oil droplet are
90nm is uniformly dispersed, and without aggregation between oil droplet, through 5000rpm, 30min centrifugation stable testing is not stratified, 50 DEG C, -10 DEG C of environment
Lower preservation three months not stratified, non-discolouring.
Embodiment 5:
A kind of preparation method of sulforaphen pik woods micro emulsion, it is characterised in that use following steps:
A, weigh raw material according to following mass ratio: 2.0% zeins, 0.5% corn glycogen, 0.10% sodium chloride,
12.0% ethyl alcohol, 18.0% ring five dimethyl silicone polymer, 13.5% methyl pyrrolidone, 4.5% sulforaphen, 4.0% isononanoic acid are different
Nonyl ester, 2.4% samara oil, 2.4% jojoba oil, 0.50% Phenoxyethanol, surplus are distilled water；
B, by zeins and ethyl alcohol, emulsion pot is put into, is stirred at room temperature with 180rpm speed to being completely dissolved,
Then load weighted distilled water, corn glycogen are put into, is stirred at room temperature with 400rpm speed to being completely dissolved, is eventually adding chlorination
Sodium, Phenoxyethanol, obtain aqueous dispersion liquid, are adjusted to the pH value of aqueous dispersion liquid using citric acid-sodium citrate buffer solution
6.8；
C, sulforaphen and methyl pyrrolidone are added to oily phase pot, five polydimethylsiloxanes of ring is added after being dispersed with stirring
Alkane, isononyl isononanoate, samara oil, jojoba oil obtain miscella phase；
D, gained miscella phase in step C is mixed in emulsion pot with aqueous dispersion liquid obtained by step B, with 500rpm's
Revolving speed stirs 30min, obtains sulforaphen pik woods premixed solution；
E, gained sulforaphen pik woods premixed solution in step D is put into high pressure homogenizer, at room temperature in 1000bar
Homogeneous 7 times under (100MPa) pressure, each homogeneous 6min obtain sulforaphen pik woods microemulsion.
Sulforaphen Pickering microemulsion pH value 6.60, rotary viscosity 3500cps obtained by the present embodiment
(Brookfield viscosimeter, 2# rotor, revolving speed 6RPM), sulforaphen drugloading rate 4.20wt%, the average-size of oil droplet are
68nm is uniformly dispersed, and without aggregation between oil droplet, through 5000rpm, 30min centrifugation stable testing is not stratified, 50 DEG C, -10 DEG C of environment
Lower preservation three months not stratified, non-discolouring.
Zeins used is purchased from Shandong Rui Feng sugar industry Co., Ltd in embodiment of the present invention, and partial size is about 40
~60nm, average molecular weight are about 30kDa；Corn glycogen (CAS 9005-79-2) is purchased from Mirexus company, and partial size is about 60
~80nm, average molecular weight are about 1500kDa；Ethyl alcohol is purchased from Shanghai Aladdin biochemical technology limited liability company, analyzes pure, matter
Measure score 92.0%；Sodium chloride, citric acid-sodium citrate buffer solution are purchased from Shanghai Aladdin biochemical technology limited liability company,
Purity is higher than 99%；Phenoxyethanol (CAS 122-99-6) is purchased from GALAXY company, India；Sulforaphen (CAS 142825-10-
3) Hangzhou Lin Gebei Science and Technology Ltd., content 98% are purchased from；Methyl pyrrolidone is purchased from the limited public affairs of good method lion (Shanghai) trade
Department, purity are higher than 99.8%；Isononyl isononanoate is purchased from BASF Corp. of Germany；Ring five dimethyl silicone polymer is purchased from Japanese SHIN-ETSU HANTOTAI
Organosilicon；High pressure homogenizer used is purchased from Sea Bream jump precision machinery trade Co., Ltd, model M-110EH；Emulsion pot used
For the vacuum emulsification pot for being purchased from her German Ka Tuo company, model EKATO LM6,50L；PH meter used is purchased from plum Teller-support benefit
(METTLER TOLEDO) international trade (Shanghai) Co., Ltd., model Seven Compact；Rotational viscometer used is purchased from beauty
BROOKFIELD company, state, model DV-II+ Pro；High performance liquid chromatographs used has purchased from Agilent Technologies (China)
Limit company, model Agilent 1260；Centrifuge used is purchased from German Sigma, model sigma1-14.
Claims (2)
1. a kind of sulforaphen pik woods micro emulsion, it is characterised in that: including following components: 1.2~2.5% zeins,
0.3~0.6% corn glycogen, 0.02~0.12% sodium chloride, 5.0~15.0% ethyl alcohol, 12.0~25.0% ring five are poly-
Dimethyl siloxane, 4.8~13.5% methyl pyrrolidone, 3.0~5.0% sulforaphen, 3.0~8.0% isononanoic acid it is different
Nonyl ester, 2.0~5.0% vegetable oil, 0.50% Phenoxyethanol, surplus are distilled water, and the percentage is mass percent.
2. the preparation method of sulforaphen pik woods micro emulsion described in claim 1, it is characterised in that use following steps:
A, weigh raw material according to following mass ratio: 1.2~2.5% zeins, 0.3~0.6% corn glycogen, 0.02~
0.12% sodium chloride, 5.0~15.0% ethyl alcohol, 12.0~25.0% ring five dimethyl silicone polymers, 4.8~13.5% crassitudes
Ketone, 3.0~5.0% sulforaphens, 3.0~8.0% isononyl isononanoates, 2.0~5.0% vegetable oil, 0.50% Phenoxyethanol, surplus
For distilled water；The vegetable oil is avocado oil, linseed oil, white pond flower seed oil, hippophae rhamnoides fruit oil, camellia seed oil, wheat embryo
One of oil, samara oil, jojoba oil or their mixture；
B, by the zeins and ethyl alcohol, emulsion pot is put into, is stirred at room temperature with 100~200rpm speed to complete
Dissolution, then put into the distilled water, corn glycogen, stirred at room temperature with 300~450rpm speed to being completely dissolved, finally plus
Enter the sodium chloride, Phenoxyethanol, obtain aqueous dispersion liquid, citric acid-sodium citrate buffer is added by the water phase point
The pH value of dispersion liquid is adjusted to 6.0~7.0；
C, the sulforaphen and methyl pyrrolidone are added to oily phase pot, five poly dimethyl of ring is added after being dispersed with stirring
Siloxanes, isononyl isononanoate, vegetable oil obtain miscella phase；
D, gained miscella phase in step C is mixed in emulsion pot with aqueous dispersion liquid obtained by step B, with 500~650rpm
Revolving speed stir 30min, obtain sulforaphen pik woods premixed solution；
E, gained sulforaphen pik woods premixed solution in step D is put into high pressure homogenizer, at room temperature in 1000bar pressure
Lower homogeneous 5~10 times, each 3~8min of homogeneous obtain sulforaphen pik woods microemulsion.
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