CN110215415A - Low viscous submicron emulsion of one kind and the preparation method and application thereof - Google Patents
Low viscous submicron emulsion of one kind and the preparation method and application thereof Download PDFInfo
- Publication number
- CN110215415A CN110215415A CN201910349925.XA CN201910349925A CN110215415A CN 110215415 A CN110215415 A CN 110215415A CN 201910349925 A CN201910349925 A CN 201910349925A CN 110215415 A CN110215415 A CN 110215415A
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- Prior art keywords
- oil
- submicron emulsion
- low viscous
- homogeneous
- emulsion
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Classifications
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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
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- A61K8/04—Dispersions; Emulsions
- A61K8/06—Emulsions
- 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
- A61K8/31—Hydrocarbons
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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
- A61K8/60—Sugars; Derivatives thereof
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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
- A61K8/671—Vitamin A; Derivatives thereof, e.g. ester of vitamin A acid, ester of retinol, retinol, retinal
-
- 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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- 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
- A61K8/678—Tocopherol, i.e. vitamin E
-
- 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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/86—Polyethers
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- 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
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
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Abstract
The invention discloses a kind of low viscous submicron emulsions and the preparation method and application thereof, and low viscous submicron emulsion is made of the raw material of following mass percentage through super-pressure nanometer homogeneous: 1) water and water soluble ingredient 35%~99.5%;2) moisturizing grease 0.1%~30%;3) oil-soluble active UV absorption indicator substance 0.1%~15%;4) surfactant 0.1%~15%;5) preservative 0.2%~5%;The sum of mass percent of said components is 100%.Preparation method is included the following steps: to prepare water phase and oily phase respectively, be obtained using extra-high-pressure nano homogenizer emulsifying.Low viscous submicron emulsion contains various high-efficiency activated skin care ingredients, in the cosmetics applied to different systems, so that making an addition to active skincare substance in cosmetics is able to the effect of playing its active skincare, and with scientific its effective skin care of method validation.
Description
Technical field
The present invention relates to a kind of cosmetics, skin care item technology, more particularly to a kind of low viscous submicron emulsion and preparation method thereof
With application, a kind of skin care item of low viscous submicron emulsion system are such as prepared, a kind of active skincare group of submicron emulsion can also be prepared
Point, it makes an addition in all kinds of skin care item.
Background technique
As the cosmetology consciousness of people is also gradually increased, demand of the consumer to cosmetics is more and more, selection
It is more and more, and require more and more, have to product efficacy and more and more specifically more clearly require, to product appearance and skin sense
Etc. sensory experiences also increasingly pay attention to.The slim and graceful luxurious effect skin care item of skin sense come into being.Such skin care quality sense is salubrious, easily
By percutaneous absorption, there is special nursing role to skin.
In addition to safety, the also concern increasingly by consumer and manufacturer of the validity of cosmetics." cosmetics
Effect declares verification guide principle " (exposure draft) to effect declare verifying principle, method and all elements carried out it is bright
Really specification.During cosmetic industry fast development, the function subdivision trend of product is more obvious, cosmetic industry evaluation
It is to its both effectiveness effective means for declaring to carry out scientific support, essence is to declare to provide corresponding card for the effect of cosmetics
According to and foundation.By the development evolvement of many years, gradually perfect, the national prison of China safety evaluation of cosmetics system
Also gradually thus preceding product hygienic quality of focusing on is transferred to concern Product quality and safety to management thought, and measuring means is also experiencing
From traditional product toxicology test to reinforcement raw materials control, carries out more scientific risk assessment and introduce substitution detection method
Transformation.Cosmetic industry evaluation can be by a variety of methods such as biochemistry, cell biology, clinical evaluation to cosmetic industry
Carry out integration test, reasonable analysis and scientific explarnation.It is objective in addition to the experimental program for formulating scientific and precise in evaluation procedure
Evaluation appts also become essential a part in appraisal.Common effect detection has whitening, crease-resistant, anti-aging, tight
The effect of skin and other effects skin care item is caused to be detected.
Product efficacy passes through active skincare ingredients progress Transdermal absorption and plays a role to realize validity of products, and active
The percutaneous absorbtion amount and percutaneous absorbtion rate of skin care ingredient are then particularly important.The cuticula of epidermis is the main screen of Transdermal absorption
Barrier, foreign bodies through cuticula speed be also percutaneous absorbtion main rate-limiting step.In general, molecular weight is less than 300,
Positively charged substance is easy to permeate if having both fat-soluble and certain water solubility.As azone substance can improve cuticula
Percutaneous absorbtion rate can be greatly improved in permeability.The percutaneous absorbtion of functional component is more, and product effect is better, and product efficacy obtains most
The performance of limits.
Under normal circumstances, influence the factor of percutaneous absorbtion: (1) depend on transdermal substance itself characteristic: as molecular weight,
Polarity, the fat-soluble and factors such as water-soluble;(2) cuticula has storage cavern effect to the substance of percutaneous absorbtion, can store moieties,
These substance a part will be slowly absorbed, and another part will be rinsed or be taken away by skin friction;(3) matrix dosage form exists
The absorption process of transdermal substance is influenced to a certain extent: the 1. influence to skin hydration effect: cuticula energy under certain condition
Continue excessive absorption moisture, referred to as aquation.Water imbibition matrix and emulsified bases have water suction and water signature, be easy with
Skin secretion mixing, emulsification, are conducive to cuticula and are in hydration status, weaken its barrier action;2. the affinity with matrix
Power: it when matrix is big with transdermal substance affinity and forms soluble complex, discharges and slows down from matrix;On the contrary then affinity
Small, release is accelerated, and absorbs and increases;3. transdermal substance and skin contact area: in two-phase matrix, such as oil-in-water type or Water-In-Oil
Type, it is necessary to enable nutrient to have higher distribution coefficient in foreign minister, so that the substance can be conducive to skin surface close contact
It absorbs.4. the pH value of matrix can influence the percutaneous absorbtion of weak electrolyte, when matrix pH value is less than the pKa of acidic materials or is greater than alkali
Property object pKa when, which exists with molecular forms, fat-soluble to become larger, and is conducive to absorb.
Submicron emulsion submicron emulsion (SE), partial size in the new emulsion for 0.1 μm~1 μm, have compared with
High load medicine and encapsulation rate, by using Submicron Emulsion as active carrier, it is intended to prepare a kind of with partial size appropriate, biology benefit
Expenditure is high, good absorbing, safety and stability, bland New Emulsion, and a new way efficiently, safe can be opened up for skin care item
Diameter.
Summary of the invention
For overcome the deficiencies in the prior art, one of the objects of the present invention is to provide a kind of low viscous submicron emulsions, containing each
The high-efficiency activated skin care ingredient of kind.
The second object of the present invention is to provide a kind of ultralow viscous submicron emulsion containing various high-efficiency activated skin care ingredients
The preparation method of system in the cosmetics applied to different systems, is sent out so that making an addition to active skincare substance in cosmetics
The effect of waving its active skincare.
The third object of the present invention is to provide a kind of low viscous submicron emulsion Transdermal absorption in skin care item, cosmetics and answers
With method, using its effective skin care of the method validation of science.
An object of the present invention adopts the following technical scheme that realization: a kind of low viscous submicron emulsion, by following quality percentage
The raw material of number meter is made through super-pressure nanometer homogeneous:
The sum of mass percent of said components is 100%.
Further, the water soluble ingredient is in chelating agent, single or polyols blend, water-soluble actives
The composition of one or more kinds of arbitrary proportion mixing.
Further, the moisturizing grease be selected from Sucrose acetoisobutyrate, castor bean, Castor oil, jojoba seed oil,
Olive oil, Queensland nut seed oil, olive oil, saualane, avocado oil, grape seed oil, sunflower oil, dog rose fruit oil,
Lavender oil, Prunus Amygdalus Dulcis Oil, oat kernel oil, thorn A Ganshu benevolence oil, granada seed oil, azadirachta seed be oily, one in white pond flower seed oil
Kind or the composition of two or more arbitrary proportions mixing.
Further, the oil-soluble active UV absorption indicator substance is selected from vitamin A derivatives, tocopherol, fertility
The combination of one or more of phenol acetic acid esters, vitamine C palmitate, ascorbyl palmitate arbitrary proportion mixing
Object.
Further, the surfactant is selected from rilanit special 40, rilanit special 60, PPG-26- butylol polyether-
26, the composition of one or more of solubilizer LRI arbitrary proportion mixing.
Further, the preservative be selected from methyl hydroxybenzoate, Phenoxyethanol, Sensiva SC50, benzyl alcohol, pentanediol,
The composition of one or more of hexylene glycol, pungent glycol, olein arbitrary proportion mixing.
The second object of the present invention adopts the following technical scheme that realization: a kind of preparation method of low viscous submicron emulsion, including
Following steps:
1) water and water soluble ingredient of formula ratio under room temperature, is added, is dispersed with stirring and dissolves, forms system A;
2) moisturizing grease, oil-soluble active UV absorption indicator substance and the surface under room temperature, adding formula ratio are living
Property agent, stir evenly, formed system B;
3) system B is added in system A room temperature, stirs homogeneous, and emulsification is uniform;Or system A, B is separately heated to 75
~80 DEG C, homogeneous is stirred, uniformly, it is stand-by that room temperature is down in stirring for emulsification;The preservative for finally successively adding formula ratio again, obtains general
Logical homogeneous lotion;
4) it uses extra-high-pressure nano homogenizer emulsifying: setting the condition of extra-high-pressure nano homogenizer, received with super-pressure
Rice homogenizer carries out homogeneous to common homogeneous lotion obtained by step 3), to prepare low viscous submicron emulsion.
Further, it is 20 DEG C that the condition of the step 4) extra-high-pressure nano homogenizer, which is the temperature of cooling water circulation,;If
Determine host high-pressure pump: 1500bar, low pressure automatic adjustment are as follows: 32/33bar.
Further, it is repeated homogeneous 2-9 times using the step 4).
An object of the present invention adopts the following technical scheme that realization: the low viscous submicron emulsion of one kind is in skin care item, cosmetics
The application of middle Transdermal absorption.
Compared with prior art, the beneficial effects of the present invention are:
(1) a kind of preparation method of ultralow viscous submicron emulsion system containing various high-efficiency activated skin care ingredients is provided, is answered
In cosmetics for different systems, it is able to play the function of its active skincare so that making an addition to active skincare substance in cosmetics
Effect, and with scientific its effective skin care of method validation.Prepared by concrete application super-pressure nanotechnology a kind of low glues high-efficiency activated shield
The submicron emulsion system of skin ingredient provides a kind of Research Thinking of skin-care effect for being effectively improved daily use chemicals skin care item.Super-pressure is equal
Matter number is more, and product cut size is smaller, and the influence after homogeneous 3 times to product cut size size is little.Extra-high-pressure nano homogenizer
Condition set: cooling water circulation temperature as 20 DEG C;Set host high-pressure pump: 1500bar, low pressure automatic adjustment are as follows: 32/
33bar, to prepare super-pressure nanometer homogeneous lotion.
(2) through experimental exploring it is found that preparing the proportion that stable submicron emulsion key is oily phase and surfactant, i.e.,
The grease and water-soluble substances of equivalent, the surfactant of addition is more, and the partial size of lotion is smaller more stable.The molten substance of oil it is total
Content is within 3 times of surface-active contents or when lower loading, and the partial size of available solution is smaller, more concentrates, is steady
Fixed submicron emulsion.Because emulsifier is bigger, the micella of formation is more, and emulsion particle is also more, and latex particle size is got over
It is small.
Although ordinary emulsion can obtain stable submicron emulsion by adding more surfactants, addition is more
Surfactant, formulation cost increases, and the irritation of product also increases, and particle diameter distribution is still relatively wide, but receives by super-pressure
Rice homogenizer homogenization emulsion particle diameter it is smaller, the additive amount of surfactant is lower, and product is more stable, active skincare at
The percutaneous absorbtion amount divided is higher.
(3) it finds after tested, takes the ordinary emulsion and sub-micro that the oil of ambient stable is mutually 1:1 with the proportion of surfactant
Lotion compares test, obtains the uptake and absorption rate of both;Submicron emulsion transdermal absorption factor can be than traditional cream
Liquid is high.
Detailed description of the invention
Fig. 1 is the particle diameter distribution of the common homogeneous lotion of embodiment 1;
The emulsion particle diameter that Fig. 2 is 1 extra-high-pressure nano homogenizer homogeneous of embodiment 1 time is distributed;
The emulsion particle diameter that Fig. 3 is 1 extra-high-pressure nano homogenizer homogeneous of embodiment 3 times is distributed;
The emulsion particle diameter that Fig. 4 is 1 extra-high-pressure nano homogenizer homogeneous of embodiment 5 times is distributed;
The emulsion particle diameter that Fig. 5 is 1 extra-high-pressure nano homogenizer homogeneous of embodiment 7 times is distributed;
The emulsion particle diameter that Fig. 6 is 1 extra-high-pressure nano homogenizer homogeneous of embodiment 9 times is distributed;
Fig. 7 is the emulsion particle diameter distribution of surfactant/oil phase=1/3 in the low viscous submicron emulsion of embodiment 2;
Fig. 8 is the absorbance value standard concentration curve of Retinol Palmitate;
Fig. 9 is that the external residual quantity of Retinol Palmitate changes over time curve;
Figure 10 is the external residual quantity percentage column figure of P18-1, P18-2-3 lotion;
Figure 11 is the partial size state of two kinds of lotions in the anti-ageing submicron emulsion of 3 vitamin A of example;
Figure 12 is the partial size state that 4 vitamin E of example nourishes two kinds of lotions in submicron emulsion.
Specific embodiment
In the following, being described further in conjunction with attached drawing and specific embodiment to the present invention, it should be noted that not
Under the premise of conflicting, new implementation can be formed between various embodiments described below or between each technical characteristic in any combination
Example.
In the present invention, if not refering in particular to, all parts, percentage are unit of weight, used equipment and raw material etc.
It is commercially available or commonly used in the art.Method in following embodiments is unless otherwise instructed the normal of this field
Rule method.
A kind of low viscous submicron emulsion is made of the raw material of following mass percentage through super-pressure nanometer homogeneous:
The sum of mass percent of said components is 100%.
As further preferred scheme, the water soluble ingredient is more selected from chelating agent (such as EDETATE SODIUM), single or mixing
(water soluble humectants are as urinated for first alcohol (such as dipropylene glycol, propylene glycol, sorbierite, butanediol, glycerol) and water-soluble actives
Element, ethoxy urea, trehalose, polyquaternium -51, tremella polysaccharides, Sodium Hyaluronate, carbohydrate isomer, water solubility
Extract etc.) one or more of arbitrary proportion mixing composition.
As further preferred scheme, the moisturizing grease be selected from Sucrose acetoisobutyrate, castor bean, Castor oil,
Jojoba seed oil, olive oil, Queensland nut seed oil, olive oil, saualane, avocado oil, grape seed oil, sunflower oil, dog
Tooth cynarrhodion oil, lavender oil, Prunus Amygdalus Dulcis Oil, oat kernel oil, thorn A Ganshu benevolence oil, granada seed oil, azadirachta seed oil, Bai Chihua
The composition of one or more of seed oil arbitrary proportion mixing.
As further preferred scheme, the oil-soluble active UV absorption indicator substance is selected from retinyl palmitate etc.
The vitamin e derivatives such as vitamin A derivatives, tocopherol, tocopherol acetate, vitamine C palmitate, ascorbic acid palm
The composition of one or more of acid esters arbitrary proportion mixing.
As further preferred scheme, the surfactant is selected from emulsifier (such as Sucrose Acetate acid sucrose of high hlb
Ester), one of solubilizer (such as rilanit special 40, rilanit special 60, PPG-26- butylol polyether -26, solubilizer LRI)
Or the composition of two or more arbitrary proportion mixing.
As further preferred scheme, the preservative is selected from methyl hydroxybenzoate, Phenoxyethanol, Sensiva SC50, benzene first
The composition of one or more of alcohol, pentanediol, hexylene glycol, pungent glycol, olein arbitrary proportion mixing.
It is specific embodiment of the present invention below, used raw material, equipment etc. remove special limit in the following embodiments
It can be obtained by buying pattern outside fixed.
A kind of embodiment 1: low viscous submicron emulsion
Table 1 is the formula composition of the low viscous submicron emulsion of embodiment 1
Standard Chinese name | Mass percentage % |
Water | 79.7 |
Butanediol (water soluble ingredient) | 8 |
Retinyl palmitate (oil-soluble active UV absorption indicator substance) | 0.1 |
Sucrose acetoisobutyrate (moisturizing grease) | 2.9 |
Castor-oil plant (Ricinus Communis) seed oil (moisturizing grease) | 5 |
Solubilizer LRI (surfactant) | 4 |
Methyl hydroxybenzoate (preservative) | 0.3 |
Note: the INCI title of solubilizer LRI: Cremophor RH40/- 26/ water of PPG-26- butylol polyether
A kind of embodiment 2: low viscous submicron emulsion
Table 2 is the formula composition of the low viscous submicron emulsion of embodiment 2
Note: the INCI title of solubilizer LRI: Cremophor RH40/- 26/ water of PPG-26- butylol polyether
The formula of embodiment 2 and embodiment 1 be formulated the difference is that only lipophilic component content is different, form 3 emulsion systems
(being shown in Table 2), each system complete step 1) -3 in preparation method), common homogeneous emulsion fraction storage sample, remaining major part is made
The extra-high-pressure nano homogenizer emulsifying for carrying out step 4), is repeated 3 times, and test result comparison is shown in Table 4.
The preparation method of the low viscous submicron emulsion of embodiment 1-2, includes the following steps:
1) water and water soluble ingredient of formula ratio under room temperature, is added, is dispersed with stirring and dissolves, forms system A;
2) moisturizing grease, oil-soluble active UV absorption indicator substance and the surface under room temperature, adding formula ratio are living
Property agent, stir evenly, formed system B;
3) system B is added in system A room temperature, stirs homogeneous, and emulsification is uniform;Or system A, B is separately heated to 75
~80 DEG C, homogeneous is stirred, uniformly, it is stand-by that room temperature is down in stirring for emulsification;The preservative for finally successively adding formula ratio again, obtains general
Logical homogeneous lotion;It leaves and takes part and is used as test;
4) it uses extra-high-pressure nano homogenizer emulsifying: setting the condition of extra-high-pressure nano homogenizer: cooling water circulation
Temperature be 20 DEG C;Setting host high-pressure pump: 1500bar (can beat) in operation between 1460~1536, low pressure automatic adjustment
Are as follows: 32/33bar;Homogeneous, homogeneous 0-9 are carried out to common homogeneous lotion obtained by step 3) with extra-high-pressure nano homogenizer
It is secondary, to prepare low viscous submicron emulsion.
5) it takes out step 3) and 4) resulting partial emulsion carries out centrifugal stability test, centrifugal condition: centrifugation rate
3000r/min, length of testing speech 30min, quickly judge emulsion intercalation method;
6) step 3) and 4) resulting partial emulsion are taken out and carries out partial size with Bettersize2000B laser fineness gage
Distribution tests quickly judge the particle diameter distribution situation of lotion.
The effect assessment and performance detection of embodiment 1-2
1. detecting to the performance of the low viscous submicron emulsion of embodiment 1, detection project and result are referring to table 3 and Fig. 1-
6。
The change of size comparison of the different homogenization cycles of table 3
Step 3) is prepared into above-mentioned formula system, i.e., it is ordinary emulsion that homogenization cycles, which are 0 gained, using super-pressure nanometer
Low viscous submicron emulsion obtained by homogenizer emulsifying, discovery super-high-pressure homogenization number is more, and product cut size is smaller (being shown in Table 3), grain
Diameter change procedure is shown in Fig. 1-6, it is known that the influence after homogeneous 3 times to product cut size size is little.
It as shown in figures 1 to 6, is the change of size mistake with a batch of common homogeneous lotion and super-pressure nanometer homogeneous lotion
Journey, it is known that common homogeneous emulsion particle diameter is larger relatively to be dispersed, and is more concentrated by the more partial sizes of extra-high-pressure nano homogenizer homogenization cycles
The analysis offset small toward partial size.
2. the performance of the low viscous submicron emulsion of pair embodiment 2 detects, detection project and result are referring to table 4.
The state vs of 4 different content surface active agent emulsions of table
As shown in Table 4, when surfactant/oil phase=1/1, common low viscous emulsion particle diameter is larger, super-pressure nanometer homogeneous
Emulsion particle diameter is smaller more to be concentrated;When the molten active matter of oil is 2 times of surfactant or higher ratio, common low slimy milk liquid is unstable
It is fixed, super-pressure nanometer homogeneous emulsion-stabilizing, it is known that the shakiness of low level of surfactant can be made using extra-high-pressure nano homogenizer
Determine lotion to become stable, it is possible to reduce the application of lotion Surfactant.
3. 3 sections of nanometer homogeneous lotions (homogeneous 3 times) obtained by pair embodiment 2, with Bettersize2000B laser particle size
Distribution instrument carries out particle diameter distribution test, quickly judges the particle diameter distribution situation of lotion, as a result as follows:
The partial size of 5 different content surface active agent emulsions of table compares
Tested above it is found that the total content of the molten substance (moisturizing grease) of oil be within 3 times of surface-active contents or
When lower loading, the stable submicron emulsion that its partial size of lotion smaller (being shown in Table 5) more concentrates (see Fig. 7) can be obtained.(when the molten object of oil
When the total content of matter is 4 times of surfactant, obtained emulsion particle diameter is not in the range of submicron emulsion, not as ours
Research object)
In conclusion by table 2, table 4 and table 5 it is found that the molten active material of oil and water-soluble object of equal volume in embodiment 2
Matter can be such that the unstable lotion of low level of surfactant becomes stable, can reduce cream using extra-high-pressure nano homogenizer homogeneous
The application of liquid Surfactant reduces formulation cost and the stimulation of surfactant bring, obtains the smaller milder of partial size more
Stable lotion.
4. characterizing the percutaneous absorptivity of submicron emulsion
Vitamin is commonly used in skin care item and its derivative carrys out skin care, and the bioactivity of vitamin A is mainly reflected in maintenance machine
A variety of skin care anti-aging functions, the vitamin Es such as growth, the complete, inhibition of lipid peroxidation of maintenance epidermis of body have anti-aging, resist
Peroxidating and the effect of ultraviolet injury resistant.The oil that vitamin A derivatives or vitamin e derivative etc. have UV absorption can be added
Melt into point is prepared into submicron emulsion, and carries out percutaneous penetration.This test object (is also known as regarded with Retinol Palmitate
Flavol palmitate) for, including following characteristics content:
A, prepare the standard solution of Retinol Palmitate: 10.00 μ g/mL Retinol Palmitate standards of selection are molten
Liquid carries out ultraviolet absorption peak scanning with ultraviolet permeability analyzer UV-2000S in 400-220nm wave-length coverage, obtains it most
Big absorbing wavelength is 326nm;The absorbance value under 326nm is read, Retinol Palmitate absorbance value-mass concentration is drawn
Curve, obtained Retinol Palmitate standard curve are y=0.0866x-0.00112, R2=0.998.
B, position first is chosen in experimenter's forearm health skin, having a size of 4cm2Square, it is with cotton swab that lotion is uniform
It is applied in sampling range, makes the coating weight 0.020g of lotion;
C, sample time is 0.5h, 1h, 1.5h, 2h, after reaching sample time, not with adhesive tape removing corresponding sample range
Absorbed lotion;
D, adhesive tape is put into the air-tight bottle of brown after removing, accurately pipettes 25.00mL dehydrated alcohol into air-tight bottle, is used
SK1200E ultrasonic cleaner ultrasound 30min;
E, the external residual lotion that elution is gone out with adhesive tape avulsion, obtains a series of samples to be measured, with ultraviolet permeability point
Analyzer UV-2000S measures absorbance value of the sample liquid at 326nm.
In this experiment, the formula of the low viscous submicron emulsion of vitamin A is as follows:
The low viscous submicron emulsion formula table of 6 vitamin A of table
Standard Chinese title | Content % |
Water | 83.65 |
Butanediol (water soluble ingredient) | 8 |
EDETATE SODIUM (water soluble ingredient) | 0.05 |
Castor-oil plant (Ricinus Communis) seed oil (moisturizing grease) | 3 |
Retinyl palmitate (oil-soluble active UV absorption indicator substance) | 1 |
- 26/ water of Cremophor RH40/butylol polyether (surfactant) | 4 |
Methyl hydroxybenzoate (preservative) | 0.3 |
The experiment carries out percutaneous absorbtion simulation test, same formula system system using Retinol Palmitate as identifying object
The ordinary emulsion obtained is labeled as P18-1, is labeled as P18- with by 3 obtained submicron emulsions of extra-high-pressure nano homogenizer homogeneous
2-3 verifies the Transdermal absorption situation of the active constituent of two lotion.
The process of percutaneous absorbtion simulation test:
1) it prepares the standard solution of Retinol Palmitate: accurately weighing the Retinol Palmitate standard specimen of certain mass
In beaker, appropriate dehydrated alcohol dissolution is added.Be made into mass concentration be 6.00 μ g/mL, 7.00 μ g/mL, 8.00 μ g/mL,
9.00 μ g/mL, 10.00 μ g/mL standard solution.
2) 10.00 μ g/mL Retinol Palmitate standard solution are selected, are existed with ultraviolet permeability analyzer UV-2000S
Ultraviolet absorption peak scanning is carried out in 400-220nm wave-length coverage, obtains a length of 326nm of maximum absorption wave;
3) with the absorbance of the Retinol Palmitate reference substance of purple light spectrophotometric determination known concentration, abscissa
For the concentration of reference substance, ordinate is absorbance, reads the absorbance value under 326nm, fits standard according to the result measured
Concentration curve, obtained regression equation are as follows: A=0.0866C-0.00112, R2=0.998.It is as shown in Figure 8 to draw standard curve.
4) before doing serial experiment, we choose t=0.5h carry out preliminary experiment, find the Transdermal absorption time in 0.5h,
The Transdermal absorption percentage difference of P18-1 and P18-2-3 lotion is 1.5% or so, therefore in subsequent serial experiment, inhaling
It is appropriately extended between time receiving, chooses 0.5h, 1h, 1.5h, 2h respectively and tested as soak time.
5) sampling point is chosen in experimenter's forearm, having a size of 4cm2Square, lotion is uniformly applied to sampling with cotton swab
In range, make the coating weight 0.020g of lotion, sample time 0.5h, 1h, 1.5h, 2h, after reaching sample time, uses adhesive tape
The unabsorbed lotion of corresponding sample range is removed, adhesive tape is put into the air-tight bottle of brown after removing, accurately pipettes 25.00mL
Dehydrated alcohol is into air-tight bottle, with SK1200E ultrasonic cleaner ultrasound 30min, external residual of the elution with adhesive tape avulsion out
Lotion obtains a series of samples to be measured, measures absorbance value of the sample liquid at 326nm.
Test result: as shown in Figure 9, the active matter of same concentrations is within the identical testing time, the external residual of P18-1
Concentration is higher, i.e., less by the skin care ingredient of percutaneous absorption;As shown in Figure 10, in the identical testing time, P18-2-3's is external
Residual volume percentage ratio P18-1 is small, illustrates in the same testing time, and the absorption rate of P18-2-3 is larger, and from figure
In as can be seen that 1h to 1.5h during P18-2-3 residual quantity percentage decline amount ratio P18-1 it is more, illustrate this section survey
It tries in the time, the absorption rate ratio P18-1's of P18-2-3 is big.
The anti-ageing submicron emulsion of 3 vitamin A of embodiment
The low viscous submicron emulsion formula table of 7 embodiment of table, 3 vitamin A
Standard Chinese name | Mass percentage % |
Water (purified water or deionized water) | 81.65 |
EDETATE SODIUM (chelating agent in water soluble ingredient) | 0.05 |
Butanediol (water soluble ingredient) | 8 |
Retinol Palmitate (oil-soluble active UV absorption indicator substance) | 1 |
Castor oil (moisturizing grease) | 3 |
Castor-oil plant (Ricinus Communis) seed oil (moisturizing grease) | 5 |
Solubilizer LRI (surfactant) | 1 |
Methyl hydroxybenzoate (preservative) | 0.3 |
Note: the INCI title of solubilizer LRI: Cremophor RH40/- 26/ water of PPG-26- butylol polyether
The anti-ageing submicron emulsion of vitamin A the preparation method is as follows:
1. a suitable vessel is added in 1,3-BDO, EDETATE SODIUM and water, it is heated to 80-85 DEG C, is dissolved by heating completely,
It stirs evenly, is labeled as water phase, keep the temperature spare.
2. a suitable vessel is added in castor oil, Retinol Palmitate and solubilizer LRI, it is heated to 80-85 DEG C, is added
Thermal agitation is uniform, is labeled as oily phase, keeps the temperature spare.
3. under appropriate shearing condition, during the oil phase is added to the aqueous phase, stirs emulsifying 10 minutes, stop homogeneous, stirring
It is cooling.
4. be cooled to 40 DEG C hereinafter, allotment terminate, finally successively add methyl hydroxybenzoate again, obtain common homogeneous lotion;It takes
A part is labeled as ordinary emulsion P18-1 out, uses for contrast test.
5. use extra-high-pressure nano homogenizer, set temperature that cooling water starts the cycle over as 20 DEG C, setting host condition: height
Press pump: 1500bar, low pressure automatic adjustment are as follows: 32/33bar cleans extra-high-pressure nano homogenizer with purified water, then will be above-mentioned
The resulting ordinary emulsion of step pours into, and beginning is high-pressure homogeneous, and homogeneous resulting lotion early period is outwelled, and a clean container is taken to hold institute
The lotion obtained.The step repeats repeatedly, and submicron emulsion is made.
The effect assessment and performance detection of embodiment 3
1. centrifugation test
Equipment: instrument title: DTL-A- type desk centrifuge, centrifugation rate and length of testing speech: 2000rpm, 30min are surveyed
Test result: ordinary emulsion and submicron emulsion pass through centrifugation test, and the two is all stable emulsion.
2. partial size is tested
Equipment: Bettersize2000B laser fineness gage
Test result: as shown in figure 11, the partial size of ordinary emulsion is bigger more dispersed, processed through extra-high-pressure nano homogenizer
Lotion partial size it is smaller more concentrate, be distributed within the scope of submicron emulsion.
4 vitamin E of embodiment nourishes submicron emulsion
8 embodiment of table, 4 vitamin E nourishes submicron emulsion formula table
The anti-ageing submicron emulsion of vitamin A the preparation method is as follows:
1. first Sodium Hyaluronate, hexylene glycol, propylene glycol are added a suitable vessel and are dispersed with stirring uniformly, purifying is added
Water is heated to 80-85 DEG C, stirs evenly, and is labeled as water phase, keeps the temperature spare.
2. a suitable vessel is added in Sucrose acetoisobutyrate, tocopherol, Phenoxyethanol and solubilizer LRI, stirring is equal
It is even, it is heated to 80-85 DEG C, is labeled as oily phase, is kept the temperature spare.
3. the oil phase is added to the aqueous phase middle emulsifying 10 minutes in the case where stirring homogeneous, stop homogeneous, stirring cooling.
4. being cooled to 40 DEG C hereinafter, allotment terminates, taking-up a part is labeled as ordinary emulsion, uses for contrast test.
5. use extra-high-pressure nano homogenizer, set temperature that cooling water starts the cycle over as 20 DEG C, setting host condition: height
Press pump: 1500bar (can beat) in operation between 1460~1536, low pressure automatic adjustment are as follows: 32/33bar is cleaned with purified water
Then extra-high-pressure nano homogenizer is poured into the resulting ordinary emulsion of above-mentioned steps, beginning is high-pressure homogeneous, and homogeneous is resulting early period
Lotion is outwelled, and a clean container is taken to hold resulting lotion.The step is repeated two more times, and submicron emulsion is made.
The effect assessment and performance detection of embodiment 3-4
1. centrifugation test
Equipment: instrument title: DTL-A- type desk centrifuge, centrifugation rate and length of testing speech: 2000rpm, 30min are surveyed
Test result: ordinary emulsion and submicron emulsion pass through centrifugation test, and the two is all stable emulsion.
2. partial size is tested
Equipment: Bettersize2000B laser fineness gage
Test result: as shown in figure 12, the partial size of ordinary emulsion is bigger more dispersed, processed through extra-high-pressure nano homogenizer
Lotion partial size it is smaller more concentrate, be distributed within the scope of submicron emulsion.
The above embodiment is only the preferred embodiment of the present invention, and the scope of protection of the present invention is not limited thereto,
The variation and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed range.
Claims (10)
1. a kind of low viscous submicron emulsion, which is characterized in that by the raw material of following mass percentage through super-pressure nanometer homogeneous system
At:
The sum of mass percent of said components is 100%.
2. low viscous submicron emulsion as described in claim 1, which is characterized in that the water soluble ingredient is selected from chelating agent, single
Or the composition of one or more of polyols blend, water-soluble actives arbitrary proportion mixing.
3. low viscous submicron emulsion as described in claim 1, which is characterized in that the moisturizing grease is selected from Sucrose Acetate acid sucrose
Ester, castor bean, Castor oil, jojoba seed oil, olive oil, Queensland nut seed oil, olive oil, saualane, avocado oil, Portugal
Grape seed oil, sunflower oil, dog rose fruit oil, lavender oil, Prunus Amygdalus Dulcis Oil, oat kernel oil, thorn A Ganshu benevolence oil, pomegranate seed
The composition of one or more of oil, azadirachta seed oil, white pond flower seed oil arbitrary proportion mixing.
4. low viscous submicron emulsion as described in claim 1, which is characterized in that the oil-soluble active UV absorption indicator substance
One in vitamin A derivatives, tocopherol, tocopherol acetate, vitamine C palmitate, ascorbyl palmitate
Kind or the composition of two or more arbitrary proportions mixing.
5. low viscous submicron emulsion as described in claim 1, which is characterized in that the surfactant is selected from rilanit special
40, one or more of rilanit special 60, PPG-26- butylol polyether -26, solubilizer LRI arbitrary proportion mix
Composition.
6. low viscous submicron emulsion as described in claim 1, which is characterized in that the preservative is selected from methyl hydroxybenzoate, benzene oxygen second
One or more of alcohol, Sensiva SC50, benzyl alcohol, pentanediol, hexylene glycol, pungent glycol, olein are any
The composition of ratio mixing.
7. a kind of preparation method of low viscous submicron emulsion, which comprises the steps of:
1) water and water soluble ingredient of formula ratio under room temperature, is added, is dispersed with stirring and dissolves, forms system A;
2) moisturizing grease, oil-soluble active UV absorption indicator substance and the surfactant of formula ratio under room temperature, are added,
It stirs evenly, forms system B;
3) system B is added in system A room temperature, stirs homogeneous, and emulsification is uniform;Or system A, B is separately heated to 75~80
DEG C, homogeneous is stirred, uniformly, it is stand-by that room temperature is down in stirring for emulsification;The preservative for finally successively adding formula ratio again obtains common equal
Matter lotion;
4) it uses extra-high-pressure nano homogenizer emulsifying: setting the condition of extra-high-pressure nano homogenizer, it is equal with super-pressure nanometer
Matter machine carries out homogeneous to common homogeneous lotion obtained by step 3), to prepare low viscous submicron emulsion.
8. preparation method as claimed in claim 7, which is characterized in that the condition of the step 4) extra-high-pressure nano homogenizer is
The temperature of cooling water circulation is 20 DEG C;Set host high-pressure pump: 1500bar, low pressure automatic adjustment are as follows: 32/33bar.
9. preparation method as claimed in claim 7, which is characterized in that repeated homogeneous 2-9 times using the step 4).
10. a kind of low viscous submicron emulsion Transdermal absorption in skin care item, cosmetics as described in any one of claims 1-9
Using.
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CN111166682A (en) * | 2020-01-17 | 2020-05-19 | 广州娇兰佳人化妆品连锁有限公司 | Micro-emulsified skin care emulsion and preparation method thereof |
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CN108498382A (en) * | 2018-06-28 | 2018-09-07 | 武汉百思凯瑞生物科技有限公司 | A kind of moisturizing conveys nano-composition and its preparation method and application altogether |
CN109453043A (en) * | 2018-12-13 | 2019-03-12 | 诺斯贝尔化妆品股份有限公司 | A kind of nanoemulsions having good stability |
CN109568178A (en) * | 2017-09-29 | 2019-04-05 | 山西远扬医药科技有限公司 | A kind of nanometer of micro emulsion composition and its nano micro-emulsification cosmetic of preparation |
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WO2000044343A1 (en) * | 1999-01-30 | 2000-08-03 | Henkel Kommanditgesellschaft Auf Aktien | Microemulsions and their use in finishing absorbent carrier substrates |
CN109568178A (en) * | 2017-09-29 | 2019-04-05 | 山西远扬医药科技有限公司 | A kind of nanometer of micro emulsion composition and its nano micro-emulsification cosmetic of preparation |
CN108498382A (en) * | 2018-06-28 | 2018-09-07 | 武汉百思凯瑞生物科技有限公司 | A kind of moisturizing conveys nano-composition and its preparation method and application altogether |
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