CN104382801B - A kind of autumn eggplant leaf flavonoids nano-emulsion and its gel for whitening spot-removing - Google Patents
A kind of autumn eggplant leaf flavonoids nano-emulsion and its gel for whitening spot-removing Download PDFInfo
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Abstract
The present invention relates to a kind of autumn eggplant leaf flavonoids nano-emulsion and its gel for whitening spot-removing, the nano-emulsion is made up of the component of following weight portion：0.3 ~ 0.65 part of autumn eggplant leaf flavonoids, 2.5 ~ 5 parts of oil phase, 1.4 ~ 6 parts of emulsifying agent, 1.4 ~ 6 parts of assistant for emulsifying agent, 40 ~ 160 parts of water, the average grain diameter of autumn eggplant leaf flavonoids nano-emulsion is less than or equal to 100nm；The gel is made up of the component of following percentage by weight：Gelatum skeleton material 0.2%~0.8%, glycerine 2%~8%, balance of autumn eggplant leaf flavonoids nano-emulsion of the invention.Autumn eggplant leaf flavonoids nano-emulsion of the invention and its gel, the autumn eggplant leaf flavonoids for using high-purity first are active component, there is the generation of suppression melanin simultaneously, suppress tyrosinase activity, anti-oxidant and uvioresistant ability, other compositions can be not required to add again can play good whitening spot-removing effect, autumn eggplant leaf flavonoids nano-emulsion and its gel stability are good, be centrifuged, high temperature, low-temperature test, it is not stratified.
Description
Technical field
The present invention relates to a kind of autumn eggplant leaf flavonoids nano-emulsion and its gel for whitening spot-removing, belong to cosmetics and its
Preparing technical field.
Background technology
Dermal melanin calmness is a kind of common multiple cutaneous disease.Including chloasma, senile plaque expelling, freckle etc., draw
The reason for playing skin melanin pigmentation is mainly human endocrine imbalance, metabolic function decrease etc., secondly Exposure to Sunlight, ultraviolet
Radiation, sleep insufficiency can aggravate pigmentation.External preparation for skin whitening spot-removing composition mainly plays a role from following approach：Suppression
Tyrosinase synthesis processed and activity, reduce skin pigment, and Chemical peeling reduces extrinsic factor such as ultraviolet, oxygen radical etc.
Negative effect to melanin physiology process.The cosmetics of current whitening spot-removing mostly have the composition of above effect respectively
Combination, the Chinese invention patent ZL's 200910037765.1 for such as having authorized discloses a kind of three integration external preparation for skin nti-freckle
Effect nanometer emulsion and preparation method thereof, describes multiple efficacies components matching in detail and plays effect of dispelling spots.
However, the whitening spot-removing composition in cosmetics in the market is generally the composition of chemical synthesis, to human body skin
There is certain excitant, security there is also certain problem.Therefore in recent years, people are more next to the quality and safety of cosmetics
More pay attention to, the cosmetics safety with natural plant extracts as main component is efficient, the trend as cosmetics exploitation.Autumn eggplant
（Kandelia candel）It is Rhizophoraceae autumn nightshade, this category only one kind, as autumn eggplant are during mangrove is classified
True mangrove plantses, the chemical composition in autumn eggplant mainly has flavonoids, tannin class, sterols, aliphatic acid and polysaccharide etc., the application's
Inventor extracts the autumn eggplant leaf flavonoids for being separated to high-purity from autumn eggplant leaf（≥60%）, show that autumn eggplant Ye is total through experimental study
Flavones is provided simultaneously with preferably suppressing melanin generation, suppresses tyrosinase activity, anti-oxidant and uvioresistant ability.Additionally, the autumn
The activity of eggplant leaf flavonoids and application there is no document report, only in the Chinese invention patent of Application No. 200610122710.7
Disclose a kind of ocean medicine hairdressing sun cream containing oyster shell powder, background technology in mention mangrove extract flavone class
Compound has very strong ultraviolet absorption ability, but in the patent and through consulting literatures, does not find any correlation test report
Road, more suppresses melanin generation, suppresses tyrosinase activity and the report for whitening cosmetics without autumn eggplant general flavone.Autumn
Eggplant leaf activity flavones is used for the invention of whitening cosmetics, is that the exploitation and deep processing of ocean Kandelia candel mangrove are established
Basis.
Epiderm skin is made up of cuticula, stratum granulosum, spinous layer, basalis, and although chloasma and other pigmentations are tables
In present face, but melanin is calm in basalis, therefore whitening spot-removing active component will be through tight heavy barrier
Basalis can be reached to play a role.The traditional formulation of cosmetics such as ordinary emulsion, cream, creme, facial mask etc., due to what is used
It is conventional art, it is impossible to ensure that active component can effectively reach basalis, and constantly play a role.And natural plants are carried
Take thing powder often to exist in the form of suspended matter in cosmetics, it is impossible to effectively dissolving dispersion, greatly limit it and penetrate skin
The ability of skin.Nano-emulsion is spontaneously formed by water, oil, surfactant and cosurfactant etc., and particle diameter is 10~100nm's
Thermodynamically stable, isotropism, transparent or semitransparent homogeneous dispersion system, easily by biomembrane, percutaneous abilities are good, can be
The reservoir of active ingredient is formed in skin, targeting, the effect of sustained release is realized.For example in Patent No. ZL200910037765.1
It is also mentioned that external application cosmetics are prepared as nano-emulsion in state's invention granted patent, but the weak point of the technical scheme exists
In：The patent all can be the monomer component for being dissolved in water phase or oil phase, and natural plant extracts are generally the mixed of Multiple components
Compound, particularly certain density ethanol extract is often all bad in water phase and oil phase solubility, make nano-emulsion difficulty compared with
Greatly.
The content of the invention
It is an object of the present invention to solve existing deficiency, there is provided a kind of autumn eggplant leaf flavonoids for whitening spot-removing
Nano-emulsion.
It is another object of the present invention to provide a kind of gel being made up of above-mentioned nano-emulsion.
The technical solution adopted for the present invention to solve the technical problems is：
A kind of autumn eggplant leaf flavonoids nano-emulsion for whitening spot-removing, is made up of the component of following weight portion：Autumn, eggplant Ye was total
0.3 ~ 0.65 part of flavones, 2.5 ~ 5 parts of oil phase, 1.4 ~ 6 parts of emulsifying agent, 1.4 ~ 6 parts of assistant for emulsifying agent, 40 ~ 160 parts of water, the autumn, eggplant Ye was total
The average grain diameter of flavones nano-emulsion is less than or equal to 100nm.
Preferably, autumn eggplant leaf flavonoids nano-emulsion is made up of the component of following weight portion：Autumn eggplant leaf flavonoids 0.4 ~ 0.6
Part, 3.5 ~ 4.5 parts of oil phase, 2 ~ 5.2 parts of emulsifying agent, 2 ~ 5.2 parts of assistant for emulsifying agent, 40~100 parts of water.
Preferably, the oil phase is isopropyl myristate；The emulsifying agent is the mixing of Tween-80 and Arlacel-80
Thing；The assistant for emulsifying agent is selected from one or more in PEG400,1,2- propane diols, glycerine.
Used as preferred, the emulsifying agent is mass ratio 1.5:1~1.9:1 Tween-80 and the mixture of Arlacel-80, help
Emulsifying agent is preferably PEG400.It is molten in several conventional oil phases that present inventor compares autumn eggplant leaf flavonoids
Xie Du, size order is isopropyl myristate>Soybean oil>Pungent certain herbaceous plants with big flowers acid glyceryl ester>Medium chain triglyceride>Ethyl oleate, because
This preferred isopropyl myristate is oil phase.Additionally, inventor has screened 1,2-PD, glycerine, PEG400, positive fourth
The emulsifying agents such as alcohol, isopropanol, find with PEG400 as assistant for emulsifying agent, are with the mixture of Tween-80 and Arlacel-80
Emulsifying agent, the nano-emulsion effect prepared after collocation is best.
It is furthermore preferred that emulsifying agent is mass ratio 1.7:1~1.8:1 Tween-80 and Arlacel-80 mixture.Due to autumn eggplant leaf
The property of general flavone is special, all bad in the solubility of water and oil phase, and to form transparent clarification has the nano-emulsion of opalescence stabilization, must
There must be the emulsifying agent of suitable HLB value, by substantial amounts of experiment sieving, emulsifying agent is used in mixed way with Tween-80 and Arlacel-80
Nano-emulsion could be formed, the mass ratio of Tween-80 and Arlacel-80 is as previously described.
Preferably, the autumn eggplant leaf flavonoids are the extract of autumn eggplant leaf, its purity is more than or equal to 60%, the autumn eggplant leaf
The extraction and purification method of general flavone is as follows：Autumn eggplant leaf coarse powder at 70 ~ 80 DEG C, with the ethanol that 15 times of volume fractions are 60%~70%
Solution is extracted 2 times, and 0.5 h, merges extract solution every time, and extract solution is concentrated to 5~6mg/L, is centrifuged, and takes supernatant, uses
HPD722 or HPD100 or HPD826 large pore resin absorption columns are purified, with the loading speed of 2 ~ 3BV/h by the supernatant of 6 ~ 7 BV
Add macroporous resin column, adsorb 30min, water-solubility impurity is washed away with the distilled water of certain volume, then with volume fraction 35%~
80% ethanol elution, elution flow rate is 3~6BV/h, and eluting agent is more than 4 BV resin column volumes, to collect eluent, wash-out
After liquid is recovered under reduced pressure solvent, vacuum or freeze-drying are crushed, and obtain final product yellowish-brown autumn eggplant leaf flavonoids.
For the preparation method of the autumn eggplant leaf flavonoids nano-emulsion of whitening spot-removing, the preparation method is as follows：By formula ratio
Emulsifying agent, assistant for emulsifying agent be placed in container, after 1 ~ 2min of magnetic agitation add formula ratio oil phase, stir 1 ~ 2min, then
The autumn eggplant leaf flavonoids of formula ratio are added, 5 ~ 8min is stirred, the water of formula ratio is finally slowly added into, continuing stirring to mixture is in
Transparence, obtains autumn eggplant leaf flavonoids nano-emulsion.
A kind of autumn eggplant leaf flavonoids nano-emulsion gel for whitening spot-removing, is made up of the component of following percentage by weight：
Gelatum skeleton material 0.2%~0.8%, glycerine 2%~8%, balance of foregoing autumn eggplant leaf flavonoids nano-emulsion.
Preferably, for whitening spot-removing autumn eggplant leaf flavonoids nano-emulsion gel by following percentage by weight component group
Into：Gelatum skeleton material is 0.3%~0.6%, glycerine 3%~6%, balance of foregoing autumn eggplant leaf flavonoids nano-emulsion.
Preferably, gelatum skeleton material is selected from Acritamer 940.
Preferably, for whitening spot-removing autumn eggplant leaf flavonoids nano-emulsion gel through being prepared from by the following method：Take
Gelatum skeleton material, adds glycerine wetting, adds autumn eggplant leaf flavonoids nano-emulsion, and 12 h are placed after stirring, fully molten
After swollen, add triethanolamine to adjust pH to 6.0 ~ 6.5, obtain final product.
The present invention has found following result by the way that autumn eggplant leaf flavonoids are carried out with activity experiment research：
（1）Influence of the autumn eggplant leaf flavonoids to B16 mouse melanin tumor cell melanin contents
From accompanying drawing 1, there is autumn eggplant leaf flavonoids significantly suppression B16 cell to make to B16 MCs
With, and with the increase of concentration, inhibiting rate gradually increases.
（2）Autumn eggplant leaf flavonoids are external to investigate result to tyrosinase inhibitory action
From accompanying drawing 2, although autumn eggplant leaf flavonoids are not so good as ascorbic acid and kojic acid to the inhibitory action of tyrosinase,
Also there is the activity of stronger suppression tyrosinase.And with the increase of concentration, inhibiting rate gradually increases.
（3）Oxidation resistance
1. autumn eggplant leaf flavonoids are to 1,1- diphenyl -2- trinitrophenyl-hydrazines（DPPH·）The Scavenging activity of free radical
As shown in accompanying drawing 3-1 and 3-2, autumn eggplant leaf flavonoids have obvious inhibitory action to DPPH, its clearance rate 0~
Rise in the concentration range of 50 μ g/mL obvious.When concentration for 50 μ g/mL clearance rates reach platform.From result, autumn eggplant leaf
The μ g/mL of general flavone 50 are to the Scavenging activity of DPPH equivalent to 20 μ g/mL ascorbic acid（Vc）.
2. autumn eggplant leaf flavonoids total phenol content is determined
Total phenol standard curve is prepared by reference substance of gallic acid, total phenol content in autumn eggplant leaf flavonoids is determined, as a result such as
Under：
Total phenol content measurement result in 1 autumn of table eggplant leaf flavonoids
As seen from Table 1, total phenol content is higher in autumn eggplant leaf flavonoids, has antioxidation activity higher polyphenol substance more,
The antioxidation activity that this also demonstrates autumn eggplant leaf flavonoids is preferable.
（4）Uvioresistant is acted on
The performance of autumn eggplant leaf flavonoids uvioresistant is investigated using the solvent method in external spf value determination method.By autumn eggplant leaf
The absorbance of 290 ~ 400 nm is determined after general flavone and the dissolving of positive control nature hall suncream, dilution, filtering, spf value is calculated.
The spf value measurement result of table 2
| Autumn eggplant concentration（µg/mL） | Spf value | Natural hall suncream concentration (μ g//mL) | Spf value |
| 25 | 2.25 | 232 | 6.04 |
| 75 | 4.18 | 348 | 16.74 |
| 125 | 13.55 | 464 | 30.76 |
From table 2, autumn eggplant leaf flavonoids have preferable uvioresistant activity.Flavones concentration is higher, and its spf value is also got over
Greatly.
A kind of autumn eggplant leaf flavonoids nano-emulsion and its gel for whitening spot-removing that the present invention is provided, its advantage
It is：
（1）Autumn eggplant leaf flavonoids nano-emulsion of the invention, the autumn eggplant leaf flavonoids that high-purity is used first are active component,
There is the generation of suppression melanin simultaneously, suppress tyrosinase activity, anti-oxidant and uvioresistant ability, can be not required to add again other into
Dividing can play good whitening spot-removing effect.
（2）Autumn eggplant leaf flavonoids nano-emulsion and its gel stability are good, are centrifuged, high temperature, low-temperature test, regardless of
Layer.
（3）The pH value of autumn eggplant leaf flavonoids nano-emulsion and its gel is 6.0 ~ 6.5, meets the weakly acidic requirement of skin.
（4）The nanoscale emulsion droplet size of formation can effectively pass through epiderm skin in 70~100nm, and stagnant in skin
Stay, improve curative effect.
（5）Nano-emulsion is made nano-emulsion gel, the viscosity of microemulsion formulation can be improved, increase the adhesion on skin,
Play slow Slow release, improve the effect of curative effect, with autumn eggplant leaf flavonoids nano-emulsion gel outward appearance obtained in Acritamer 940,
Denseness, stability etc. are most appropriate, and the pH value of the nano-emulsion gel is 6.0 ~ 6.5, and meeting that preparation for external application to skin is weakly acidic will
Ask, be centrifuged, high temperature, low-temperature test, the nano-emulsion gel is not stratified, illustrate obtained autumn eggplant leaf flavonoids nanometer curdling
Glue is stable in properties.
（6）Autumn eggplant leaf flavonoids nano-emulsion and gel man's rabbit skin and eye irritation result are illustrated as feminine gender, table
It is bright its without skin and eye irritation, use safety.
Brief description of the drawings
Fig. 1 is various concentrations autumn eggplant leaf flavonoids to B16 cell B16 cell inhibiting rate broken line graphs；
Fig. 2 is the investigation result broken line graph that autumn eggplant leaf flavonoids suppress tyrosinase in vitro；
Fig. 3-1 is Scavenging activity broken line graphs of the Vc to DPPH；
Fig. 3-2 is Scavenging activity broken line graph of the autumn eggplant leaf flavonoids to DPPH.
Specific embodiment
Below by specific embodiment, technical scheme is described in further detail.
Autumn eggplant leaf flavonoids assay uses NaNO2-Al(NO3)3- NaOH methods, concrete operations are：Diluted with 60% ethanol
With constant volume sample, 0.6 mLNaNO is added2Solution（5%）0.6 mLAl (NO are added after shaking up immediately3)3Solution（10%）, after shaking up
6 min are placed, 6 mLNaOH solution are added（1 mol/L）The mensuration absorbance at the nm of wavelength 500 immediately afterwards.
Embodiment 1：Prepare the high-purity autumn eggplant leaf flavonoids used by the present invention
（1）Extract：Take autumn eggplant leaf and be ground into meal, take 1000g, the ethanol with volume fraction 60% as extractant, solid-liquid ratio
1: 15（Mass volume ratio）, 80 DEG C of Extracting temperature, the h of extraction time 0.5, extraction 2 times.
（2）Isolate and purify：With HPD722 macroporous absorbent resins to step（1）The autumn eggplant leaf flavonoids of acquisition are purified,
Specifically purifying process is：Loading general flavone concentration is 5.0mg/mL, and loading flow velocity is 3BV/h, and applied sample amount is 6.5 BV resin columns
Volume, the min of adsorption time 30 rinses removal of impurities with 3.5 BV water, and eluant, eluent is the ethanol of volume fraction 50%, and elution flow rate is
3BV/h, eluting agent is 4 BV resin column volumes, collects ethanol, and solvent is recovered under reduced pressure, and is vacuum dried, and is crushed, and obtains Huang
Brown autumn eggplant leaf flavonoids powder 94.51g, general flavone content is 77.58%.
Embodiment 2：Prepare the high-purity autumn eggplant leaf flavonoids used by the present invention
（1）Extract：Take autumn eggplant leaf and be ground into meal, take 1000g, the ethanol with volume fraction 70% as extractant, solid-liquid ratio
1: 15（Mass volume ratio）, 70 DEG C of Extracting temperature, the h of extraction time 0.5, extraction 2 times.
（2）Isolate and purify：With HPD100 macroporous absorbent resins to step（1）The autumn eggplant leaf flavonoids of acquisition are purified,
Specifically purifying process is：Loading general flavone concentration is 6.0mg/mL, and loading flow velocity is 2BV/h, and applied sample amount is 6BV resin columns
Product, the min of adsorption time 30 rinses removal of impurities with 4BV water, and eluant, eluent is the ethanol of volume fraction 80%, and elution flow rate is 6BV/h,
Eluting agent is 4 BV resin column volumes, collects ethanol, and solvent is recovered under reduced pressure, and is vacuum dried, and is crushed, and obtains the yellowish-brown autumn
Eggplant leaf flavonoids powder 93.2g, general flavone content is 72.5%.
Embodiment 3：Prepare the high-purity autumn eggplant leaf flavonoids used by the present invention
（1）Extract：Take autumn eggplant leaf and be ground into meal, take 1000g, the ethanol with volume fraction 65% as extractant, solid-liquid ratio
1: 15（Mass volume ratio）, 78 DEG C of Extracting temperature, the h of extraction time 0.5, extraction 2 times.
（2）Isolate and purify：With HPD826 macroporous absorbent resins to step（1）The autumn eggplant leaf flavonoids of acquisition are purified,
Specifically purifying process is：Loading general flavone concentration is 4.0mg/mL, and loading flow velocity is 3BV/h, and applied sample amount is 7BV resin columns
Product, the min of adsorption time 30 rinses removal of impurities with 3BV water, and eluant, eluent is the ethanol of volume fraction 35%, and elution flow rate is 3BV/h,
Eluting agent is 4 BV resin column volumes, collects ethanol, and solvent is recovered under reduced pressure, and is vacuum dried, and is crushed, and obtains the yellowish-brown autumn
Eggplant leaf flavonoids powder 90.51g, general flavone content is 70.1%.
Embodiment 4：Prepare the autumn eggplant leaf flavonoids nano-emulsion for whitening spot-removing
Weigh Tween-80 8.4g, Arlacel-80 5.6g, PEG400 21g in glass beaker, magnetic agitation 1~
2min, adds isopropyl myristate 25g, stirs 1~2min, is subsequently adding autumn eggplant leaf flavonoids obtained in embodiment 1（Always
Flavones content is 77. 58 %）3g, stirs 5~8min, is slowly added into the water 400g of formula ratio, continues to stir always yellow to autumn eggplant Ye
The transparent shape of ketone nano-emulsion, its average grain diameter is 99.5 nm.
Embodiment 5：Prepare the autumn eggplant leaf flavonoids nano-emulsion for whitening spot-removing
Tween-80 39.31g is weighed, in glass beaker, magnetic force is stirred for Arlacel-80 20.69g, PEG400 60g
1~2min is mixed, isopropyl myristate 50g is added, 1~2min is stirred, autumn eggplant Ye obtained in embodiment 1 is subsequently adding always yellow
Ketone（General flavone content is 77. 58 %）6.5g, stirs 5~8min, is slowly added into the g of water 1600 of formula ratio, continues to stir extremely
The autumn transparent shape of eggplant leaf flavonoids nano-emulsion, its average grain diameter is 89.7 nm.
Embodiment 6：Prepare the autumn eggplant leaf flavonoids nano-emulsion for whitening spot-removing
Weigh Tween-80 12.6g, Arlacel-80 7.4g, PEG400 14g in glass beaker, magnetic agitation 1
~2min, adds isopropyl myristate 25g, stirs 1~2min, is subsequently adding autumn eggplant leaf flavonoids obtained in embodiment 1
（General flavone content is 77. 58 %）4g, stirs 5~8min, is slowly added into the g of water 1000 of formula ratio, continues to stir to autumn eggplant
The transparent shape of leaf flavonoids nano-emulsion, its average grain diameter is 85.7 nm.
Embodiment 7：Prepare the autumn eggplant leaf flavonoids nano-emulsion for whitening spot-removing
Tween-80 28.64g is weighed, in glass beaker, magnetic force is stirred for Arlacel-80 16.36g, PEG400 45g
1~2min is mixed, isopropyl myristate 40g is added, 1~2min is stirred, autumn eggplant Ye obtained in embodiment 1 is subsequently adding always yellow
Ketone（General flavone content is 77. 58 %）5g, stirs 5~8min, is slowly added into the g of water 800 of formula ratio, continues to stir to autumn eggplant
The transparent shape of leaf flavonoids nano-emulsion, its average grain diameter is 81.6 nm.
Above-mentioned autumn eggplant leaf flavonoids nano-emulsion study on the stability result：The autumn eggplant leaf flavonoids nano-emulsion of embodiment 4~7 is equal
With the min of 4000 r/min centrifugations 5, the phenomenons such as layering, precipitation, muddiness are had no, autumn eggplant leaf flavonoids nanometer milk solution is equal
Clear is kept, can be illustrated autumn eggplant leaf flavonoids nano-emulsion for O/W types and proterties is good by water infinite dilution, pH value is
6.0, meet the weakly acidic feature of preparation for external application to skin.
Embodiment 8：Prepare the gel of the autumn eggplant leaf flavonoids nano-emulsion for whitening spot-removing
Acritamer 940 0.2g is taken, the wetting of 2g glycerine is added, the autumn eggplant leaf flavonoids nano-emulsion prepared by embodiment 4 is added
97.8g, after stirring, places 12 h, after fully swelling, adds triethanolamine regulation pH, that is, obtain autumn eggplant leaf flavonoids
Nano-emulsion gel, the pH value that the autumn eggplant leaf flavonoids nano-emulsion gel is measured after being diluted with water is 6.0.
Embodiment 9：Prepare the gel of the autumn eggplant leaf flavonoids nano-emulsion for whitening spot-removing
Carbomer 9400.8g is taken, the wetting of 8g glycerine is added, the autumn eggplant leaf flavonoids nano-emulsion prepared by embodiment 5 is added
91.2g, after stirring, places 12 h, after fully swelling, adds triethanolamine regulation pH, that is, obtain autumn eggplant leaf flavonoids
Nano-emulsion gel, the pH value that the autumn eggplant leaf flavonoids nano-emulsion gel is measured after being diluted with water is 6.5.
Embodiment 10：Prepare the gel of the autumn eggplant leaf flavonoids nano-emulsion for whitening spot-removing
Acritamer 940 0.3g is taken, the wetting of 6g glycerine is added, the autumn eggplant leaf flavonoids nano-emulsion prepared by embodiment 6 is added
93.7g, after stirring, places 12 h, after fully swelling, adds triethanolamine regulation pH, that is, obtain autumn eggplant leaf flavonoids
Nano-emulsion gel, the pH value that the autumn eggplant leaf flavonoids nano-emulsion gel is measured after being diluted with water is 6.3.
Embodiment 11：Prepare the gel of the autumn eggplant leaf flavonoids nano-emulsion for whitening spot-removing
Acritamer 940 0.4g is taken, the wetting of 4g glycerine is added, is added and is prepared autumn eggplant leaf flavonoids nano-emulsion by embodiment 7
95.6g, after stirring, places 12 h, after fully swelling, adds triethanolamine regulation pH, that is, obtain autumn eggplant leaf flavonoids
Nano-emulsion gel, the pH value that the autumn eggplant leaf flavonoids nano-emulsion gel is measured after being diluted with water is 6.3.
The nano-emulsion gel of embodiment 8 to 11 carries out following study on the stability investigation：
1. centrifugal test：The g of nano-emulsion gel 5 is weighed, is placed in 10 ml centrifuge tubes, 4000 rpm are centrifuged 30 min, seen
Examine outward appearance and the stretchability change of gel.
2. low temperature resistant test：Take nano-emulsion gel appropriate, be placed in measuring cup and seal, be put into -20 DEG C of refrigerators, after 24 h
Take out, recover room temperature, the change of observation outward appearance, stretchability and pH value.
3. heat resistant test：Take nano-emulsion gel appropriate, be placed in measuring cup and seal, be put into 60 DEG C of baking ovens, taken after 24 h
Go out, recover room temperature, the change of observation outward appearance, stretchability and pH value.
As a result, the autumn eggplant leaf flavonoids nano-emulsion gel of embodiment 8~11 is through centrifugation, high temperature, low-temperature test, regardless of
Layer, proterties and stretchability all do not change.
Checking example 1
The autumn eggplant leaf flavonoids nano-emulsion of embodiment 5 and 7 and the autumn eggplant leaf flavonoids nano-emulsion gel of embodiment 9 and 11 enter
Row transdermal research experiment：
1st, experimental procedure：
（1）Mouse leather is standby：Healthy male white mouse (20 g or so) is taken, the hair on skin of abdomen is carefully cut off with scissors,
Draw neck to put to death, peel off skin of abdomen.The skin that will be stripped down is laid on glass plate, and cuticula is downwards, small with single back of the body blade
The heart rejects subcutaneous fat and adhesion thing, is then rinsed well repeatedly with physiological saline, is cut into appropriate size, and check skin
Integrality.Every time before experiment, the integrality of mouse skin is checked, there must not be any breakage.
（2）Permeation test in vitro：Using improved Franz diffusing cells method, the mouse part skin that will be handled well is fixed on supply
Between pond and acceptance pool, upwards, effective transdermal area is 3.14 cm2 to stratum corneum side.Reception liquid is physiological saline, volume 10.4
mL.1 mL is sampled respectively at 1,2,4,6,8,10,12,24 h after sample-adding, is supplied with physiological saline, sample NaNO2-Al
(NO3)3- NaOH complexometries determine general flavone content.
2nd, experiment conclusion
The autumn eggplant leaf flavonoids nano-emulsion of embodiment 5 measures micro flavones content in the sample that 6 h are passed through, embodiment 7
Autumn eggplant leaf flavonoids nano-emulsion measures micro flavones content, the autumn eggplant leaf flavonoids nano-emulsion of embodiment 9 in the sample that 8 h are passed through
Through colour developing all without flavones content, the autumn eggplant leaf flavonoids nano-emulsion gel of embodiment 11 exists the sample that gel takes in 1 ~ 12 h
The sample taken in 1 ~ 16 h, all without flavones content, illustrates that medicine is no during this period or very little passes through skin through colour developing
Skin, thus cannot be detected using ultraviolet spectrophotometry；So thus judge, autumn eggplant leaf flavonoids nano-emulsion and nanometer curdling
Glue is more long in the skin holdup time, and nano-emulsion gel adherence is strong, and the holdup time in skin is longer.
Embodiment described above is a kind of preferably scheme of the invention, not makees any formal to the present invention
Limitation, also has other variants and remodeling on the premise of without departing from the technical scheme described in claim.
Claims (8)
1. a kind of autumn eggplant leaf flavonoids nano-emulsion for whitening spot-removing, it is characterised in that be made up of the component of following weight portion：
0.3~0.65 part of autumn eggplant leaf flavonoids, 2.5~5 parts of oil phase, 1.4~6 parts of emulsifying agent, 1.4~6 parts of assistant for emulsifying agent, water 40~
160 parts, the average grain diameter of the autumn eggplant leaf flavonoids nano-emulsion is less than or equal to 100nm；
The autumn eggplant leaf flavonoids are the extract of autumn eggplant leaf, and its purity is more than or equal to 60%, the extraction of the autumn eggplant leaf flavonoids
It is as follows with purification process：Autumn eggplant leaf coarse powder extracts 2 at 70~80 DEG C with the ethanol solution that 15 times of volume fractions are 60%~70%
Secondary, each 0.5h merges extract solution, and extract solution is concentrated to 4~6mg/L, is centrifuged, and supernatant is taken, using HPD722 or HPD100
Or the purifying of HPD826 large pore resin absorption columns, the supernatant of 6~7BV is added by macroreticular resin with the loading speed of 2~3BV/h
Post, adsorbs 30min, washes away water-solubility impurity with the distilled water of 3~4BV, then with the ethanol elution of volume fraction 35%~80%, wash
Separation of flow speed is 3~6BV/h, and eluting agent is more than 4BV resin column volumes, to collect eluent, and eluent is recovered under reduced pressure solvent
Afterwards, vacuum or freeze-drying, crush, and obtain final product yellowish-brown autumn eggplant leaf flavonoids；
The oil phase is isopropyl myristate；The emulsifying agent is the mixture of Tween-80 and Arlacel-80；It is described to help emulsification
Agent is selected from one or more in PEG400,1,2- propane diols, glycerine.
2. the autumn eggplant leaf flavonoids nano-emulsion for whitening spot-removing according to claim 1, it is characterised in that：By following heavy
Measure the component composition of part：0.4~0.6 part of autumn eggplant leaf flavonoids, 3.5~4.5 parts of oil phase, 2~5.2 parts of emulsifying agent, assistant for emulsifying agent 2
~5.2 parts, 40~100 parts of water.
3. the autumn eggplant leaf flavonoids nano-emulsion for whitening spot-removing according to claim 1 and 2, it is characterised in that：It is described
Emulsifying agent is mass ratio 1.5:1~1.9:1 Tween-80 and the mixture of Arlacel-80, the preferred polyethylene glycol of assistant for emulsifying agent
400。
4. the preparation side of the autumn eggplant leaf flavonoids nano-emulsion for whitening spot-removing described in a kind of claim 1-3 any one
Method, it is characterised in that：The preparation method is as follows：The autumn eggplant leaf flavonoids of formula ratio, oil phase, emulsifying agent and assistant for emulsifying agent are put
30~60min is stirred in container, the water of formula ratio is then added, continues to stir to the transparent shape of mixture, obtain autumn eggplant
Leaf flavonoids nano-emulsion.
5. a kind of autumn eggplant leaf flavonoids nano-emulsion gel for whitening spot-removing, it is characterised in that by following percentage by weight
Component is constituted：Gelatum skeleton material 0.2%~0.8%, glycerine 2%~8%, described in balance of claim 1-4 any one
Autumn eggplant leaf flavonoids nano-emulsion.
6. the gel of the autumn eggplant leaf flavonoids nano-emulsion for whitening spot-removing according to claim 5, it is characterised in that：By
The component composition of following percentage by weight：Gelatum skeleton material 0.3%~0.6%, glycerine 3%~6%, balance of claim
Autumn eggplant leaf flavonoids nano-emulsion described in 1-5 any one.
7. the gel of the autumn eggplant leaf flavonoids nano-emulsion for whitening spot-removing according to claim 5 or 6, its feature exists
In：The gelatum skeleton material is selected from Acritamer 940.
8. the gel of the autumn eggplant leaf flavonoids nano-emulsion for whitening spot-removing according to claim 5 or 6, its feature exists
In：The gel through being prepared from by the following method：Gelatum skeleton material is taken, glycerine wetting is added, autumn eggplant Ye is added always yellow
Ketone nano-emulsion, 12h is placed after stirring, fully it is swelling after, add triethanolamine adjust pH to 6.0~6.5, obtain final product.
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| CN108159102B (en) * | 2018-01-31 | 2021-02-26 | 山西医科大学 | Preparation method and application of wormwood extract nano-emulsion gel |
| CN111803445B (en) * | 2020-07-10 | 2022-06-17 | 贵州大学 | Preparation method of high-stability nano emulsion and nano emulsion gel |
| CN114452316A (en) * | 2022-01-26 | 2022-05-10 | 吉林大学 | Walnut mountain ash flavone component nanoemulsion preparation and preparation method and application thereof |
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| CN101530377A (en) * | 2009-03-11 | 2009-09-16 | 董萍 | Triad integration freckle-removing functional nano cream for skin external use and method for preparing same |
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| CN101161231A (en) * | 2006-10-13 | 2008-04-16 | 广东海洋大学 | Ocean medicine hairdressing sun cream containing shuck powder |
| CN101530377A (en) * | 2009-03-11 | 2009-09-16 | 董萍 | Triad integration freckle-removing functional nano cream for skin external use and method for preparing same |
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Effective date of registration: 20191211 Address after: 343000 6, Feng Fang, Liao Fang village, Xixi Town, Suichuan, Ji'an, Jiangxi. Patentee after: Liao Aihua Address before: 310015 College of biological and environmental engineering, Zhejiang Shuren University, 8 Shuren street, Hangzhou, Zhejiang, Gongshu District Patentee before: Zhejiang Shuren University |