Active compound and preparation method thereof and the application in cosmetics or skin care item thereof
Technical field
The present invention relates to article of everyday use technical field, particularly relate to a kind of active compound and preparation method and the application at cosmetics or skin care item thereof.
Background technology
Tryrosinase is as the key enzyme of B16 cell, and its abnormal overexpression may result in the pigmentation disease of human body, and therefore, tyrosinase inhibitor can treat pigmentation common at present. At present, the tyrosinase inhibitor added in skin-lightening cosmetic on the market mostly is synthetics, and toxic and side effects is obvious. Adopting natural origin whitening agent to prepare cosmetics is cosmetics developing direction in future. Skin aging is the natural phenomena of human body, and nowadays problem of environmental pollution is serious, and the operating pressure of people is big, lives irregular, causes that this phenomenon of skin aging is even more serious. The modal endogenous Some Circulating Factors relevant with aging course is free radical, so for defying age, scavenging free radicals is particularly important.
Therefore, the reactive composition of plants with whitening and antioxidant activity effect is developed significant in the development of cosmetics or skin care item.
Summary of the invention
In view of above-mentioned problem of the prior art, the present invention proposes a kind of active compound with whitening, antioxidant activity and preparation method thereof and the application in cosmetics or skin care item thereof.
For reaching above-mentioned purpose, the present invention by the following technical solutions:
The preparation method that the invention discloses a kind of active compound, including: the Sucus Cocois of the mass fraction respectively sugar maple resin of 50~60 parts, the Betula platyphylla Suk. myron of 10~30 parts and 10~20 parts is mixed to form mixed liquor, then described mixed liquor is sequentially carried out enzyme denaturing, clarification, refining, concentration and stable after form described active compound.
In further technical scheme, the preparation method of active compound disclosed by the invention can also have techniques below feature:
Described enzyme denaturing step includes adopting microwave that described mixed liquor carries out enzyme inactivation treatment, and the power of wherein said microwave is 300~900W, and the time is 5~10min.
Described clarification steps includes adopting ice bath that the described mixed liquor after enzyme denaturing processes is cooled to room temperature, then carries out high speed frozen centrifugation, and wherein said centrifugal speed is 18000~25000rpm, and the time is 10~15min, and temperature is 0~5 DEG C.
It is the ultrafilter membrane of 3000~5000Da that described purification step includes the described mixed liquor after clarification steps by molecular weight, collects permeate; Preferably, the material of described ultrafilter membrane is hollow-fibre membrane, polyacrylonitrile film, polychloroethylene film, polysulfone membrane, poly (ether sulfone) film, polyvinylidene fluoride film or ceramic membrane.
Described concentration step includes the described mixed liquor through purification step is carried out vacuum film concentration, wherein concentration ratio is the 1/15~1/10 of the quality of the described mixed liquor before described enzyme denaturing process step, the speed of rotation is 700~1000rpm, vacuum is below 100Pa, and temperature is 10~20 DEG C.
Described stabilizing step includes to adding stabilizer mix homogeneously in the described mixed liquor of concentration step, and the quality of described stabilizer is the 20~40% of the quality of the described mixed liquor through concentration step.
Described stabilizer is propylene glycol, 1,3 butylene glycol, the mixture of 1,2-pentanediol, wherein propylene glycol, 1,3 butylene glycol, the mixing quality ratio of 1,2-pentanediol is 3~6:1~3:1~2.
Sugar maple resin, Betula platyphylla Suk. myron and Sucus Cocois form mixed liquor after being stirred mixing at the temperature of 0~5 DEG C.
The invention also discloses a kind of active compound, be the active compound made according to preparation method described above.
The present invention there is further disclosed herein the application in cosmetics or skin care item of a kind of active compound, it is characterised in that described active compound adds in cosmetics or skin care item according to the ratio that mass fraction is 1~40%.
Sugar maple, has another name called: Acer saccharum Marsh., America Acer saccharum Marsh., and Aceraceae Acer fallen leaves megaphanerophyte, up to 40m. " whole nation Chinese herbal medicine compilation " records the root of maple and leaf can be used as medicine, and has wind-expelling pain-stopping, can be used for having a toothache, enteritis, dysentery, and bee venom sting, skin eczema etc. are controlled in stomachache, external. It is called sugar maple resin, the various mineral salinities such as sugared part containing 2~3%, aminoacid by the colourless runny solution flowed out in sugar maple trunk. Owing to sugar maple resin has flavour, also commonly use as manufacturing preserve, confection or tobacco flavoring. The sugar maple resin adopted in the present invention is taken from the effluent in sugar maple trunk in summer.
Betula platyphylla Suk. myron is the juice gathered from silver birch live standing tree spring, the birch juice delicious just gathered, and micro-sweet (healthy disease-free trees), rich in sugar, acid, trace element and aromatic substance etc. According to surveying and determination, containing 4 kinds of vitamin (VC, VB1, VB2, VH), 11 kinds of fatty acids, 18 seed amino acids and 18 kinds of trace element in birch juice. The vital movement of human body is played an important role by these materials, often drinks Sucus Betulae platyphyllae natural drink and can promote human metabolism, it is possible to anti-angiogenic hardening and resisting fatigue. Betula platyphylla Suk. myron in the present invention is taken from the effluent in Betula platyphylla Suk. trunk in spring.
Sucus Cocois is present in a kind of composite natral liquid of Cortex cocois radicis fruit intracavity, rich in various nutrients, has local flavor and the aromatic substance of uniqueness, and main component includes acids, alcohols, esters, alkane alkene class, aldehydes, ketone and phenols etc. Food industry can be used for produce numerous food, such as nata de coco, fruit wine, vinegar, ethyl acetate etc. The coconut fruit annual production of China about 28.90 ten thousand tons, Sucus Cocois abundance, but at present the research of Sucus Cocois is reported less, utilization rate is also very low, most of Cortex cocois radicis processing factories, when processing Cortex cocois radicis, are utilized except a small amount of Sucus Cocois except making refreshment drink, are disposed mostly as refuse, this had both caused environmental pollution, caused again the huge waste of resource.Therefore, Sucus Cocois is studied and is applied to household chemicals field, be there is huge economic worth. Sucus Cocois in the present invention is taken from the intracavity liquid of ripe Cortex cocois radicis.
Compared with prior art, the beneficial effects of the present invention is: preparation method of the present invention is by forming active compound by being processed preparation after sugar maple resin, Betula platyphylla Suk. myron, the mixing of Sucus Cocois three kind of plant composition, this active compound can suppress tyrosinase activity effectively, eliminate free radical, possess good antioxidation; Being applied to prepare cosmetics or skin care item by this active compound, the cosmetics obtained or skin care item, except having natural pure and fresh plant scent, also have lasting antioxidation, whitening effect.
In further scheme, three kinds of raw materials that the active compound of the present invention adopts are respectively provided with abundant oxidase, by microwave method, the enzymatic structure in three kinds of raw materials is destroyed rapidly thus losing the activity of enzyme, avoid effective ingredient easily to aoxidize and cause color burn thus affecting active compound application in terminated cosmetic, it is ensured that the stability of active compound; Preferably, mixed liquor is by the macromole impurity such as starch that the instability easily causing product and being not easy to is absorbed by the skin, polysaccharide, protein that utilize ultrafilter membrane effectively to remove in raw material, greatly remain aminoacid, mineral salt, fragrant little molecule isoreactivity composition, so that this active compound is applied in the effect of cosmetics or skin care item more preferably.
In further scheme, active compound keeps low temperature environment in preparation process, avoid the at high temperature brown stain of the sugar in raw material and affect outward appearance, thus ensure that the outward appearance of active compound and avoiding the outward appearance to cosmetics or skin care item and impact.
Accompanying drawing explanation
Fig. 1 is the fitted figure to free radical scavenging of the active compound in the embodiment of the present invention one;
Fig. 2 is the fitted figure to tyrosinase inhibition rate of the active compound in the embodiment of the present invention two;
Fig. 3 is blank sample and uses the melanin minimizing amount comparison diagram after 28 days of the formulation product in the embodiment of the present invention five and embodiment six;
Fig. 4 is blank sample and uses the L value added comparison diagram after 28 days of the formulation product in the embodiment of the present invention five and embodiment six.
Detailed description of the invention
Below against accompanying drawing and combine preferred embodiment the invention will be further described.
The preparation method that the invention provides a kind of active compound, in one embodiment, be mixed to form mixed liquor including by the Sucus Cocois of the mass fraction respectively sugar maple resin of 50~60 parts, the Betula platyphylla Suk. myron of 10~30 parts and 10~20 parts, then described mixed liquor is sequentially carried out enzyme denaturing, clarification, refining, concentration and stable after form described active compound.
In some preferred embodiments, when above-described embodiment, it is possible to adopt at least one in following optimum condition:
Described enzyme denaturing step includes adopting microwave that described mixed liquor carries out enzyme inactivation treatment, and the power of wherein said microwave is 300~900W, and the time is 5~10min.
Described clarification steps includes adopting ice bath that the described mixed liquor after enzyme denaturing processes is cooled to room temperature, then carries out high speed frozen centrifugation, and wherein said centrifugal speed is 18000~25000rpm, and the time is 10~15min, and temperature is 0~5 DEG C.
It is the ultrafilter membrane of 3000~5000Da that described purification step includes the described mixed liquor after clarification steps by molecular weight, collects permeate;Preferably, the material of described ultrafilter membrane is hollow-fibre membrane, polyacrylonitrile film, polychloroethylene film, polysulfone membrane, poly (ether sulfone) film, polyvinylidene fluoride film or ceramic membrane.
Described concentration step includes the described mixed liquor through purification step is carried out vacuum film concentration, wherein concentration ratio is the 1/15~1/10 of the quality of the described mixed liquor before described enzyme denaturing process step, the speed of rotation is 700~1000rpm, vacuum is below 100Pa, and temperature is 10~20 DEG C.
Described stabilizing step includes to adding stabilizer mix homogeneously in the described mixed liquor of concentration step, the quality of described stabilizer is the 20~40% of the quality of the described mixed liquor through concentration step, preferably, described stabilizer is propylene glycol, 1,3 butylene glycol, 1, the mixture of 2-pentanediol, wherein propylene glycol, 1,3 butylene glycol, the mixing quality ratio of 1,2-pentanediol is 3~6:1~3:1~2.
Sugar maple resin, Betula platyphylla Suk. myron and Sucus Cocois form mixed liquor after being stirred mixing at the temperature of 0~5 DEG C.
The present invention also provides for a kind of active compound, is made by the preparation method according to any one embodiment above-mentioned.
Present invention also offers the application in cosmetics or skin care item of a kind of preparation method according to any one embodiment above-mentioned prepared active compound, wherein active compound adds in cosmetics or skin care item according to the ratio that mass fraction is 1~40%.
With specific embodiment, active compound of the present invention and preparation method thereof is described further below.
Embodiment one:
A kind of active compound containing sugar maple resin, is made up of by weight following components: sugar maple resin 50 weight portion, Betula platyphylla Suk. myron 20 weight portion, Sucus Cocois 10 weight portion. Three kinds of raw materials are be 450W at microwave power after mixing under 2 DEG C of conditions in temperature, the enzyme denaturing when time is 6min; Mixed liquor after process is 20000rpm at rotating speed after utilizing ice bath to cool to rapidly room temperature, and the time is 10min, and temperature is centrifugal at 0 DEG C, and the supernatant after centrifugal is the ultrafilter membrane of 3500Da by molecular weight, obtains permeate; Permeate is 800rpm, vacuum in rotary speed is 80Pa, and temperature is that under 20 DEG C of conditions, thin film concentration, to the 1/10 of three kinds of raw material mixed liquor initial masses, obtains concentrated solution; Adding its mass fraction in concentrated solution is 25% stabilizer, is the active compound A of the present invention after conventional mixing. Its solid content is 16%-20%, can be directly appended in skin protection cosmetics. Wherein stabilizer is the mixture of propylene glycol, 1,3 butylene glycol, 1,2-pentanediol three, and the mass ratio of mixing is 3:3:1.
Following active compound A is carried out eliminates DPPH free radical aptitude tests:
1,1-diphenyl-2-trinitrophenyl-hydrazine (DPPH) is a kind of stable nitrogen center organic free radical, its stability is essentially from the steric restriction of Resonance Stabilization action and 3 phenyl ring so that the unpaired electron being clipped on wherein nitrogen-atoms can not play its due electronics and act in pairs. When free radical scavenger exists, making it absorb fade away due to single electron pairing, it is quantitative relationship that its fading extent accepts electron number with it, thus available spectrophotometer carries out quick quantitative analysis, detect free radical scavenging situation, thus evaluating the oxidation resistance of sample. Its ability clearance rate represents, clearance rate is more big, then show that its oxidation resistance is more strong.
Sample treatment: the active compound A containing sugar maple resin is light yellow transparent liquid, possesses novel aroma, when carrying out DPPH removing test experiments, is proportionally diluted to desired concn with pure water.
Test method: with dehydrated alcohol for solvent compound concentration for 2 × 10-4The DPPH alcoholic solution of mol/L; Analyte sample fluid (active compound A) 2ml is added in test tube, adds 2mlDPPH alcoholic solution, standing and reacting 30min after mixing; Absorbance is measured at 517nm place.
Each concentration tests to ensure the accuracy of experimental result in triplicate, finally averages as fitting data, and wherein the computing formula of DPPH clearance rate is as follows:
DPPH clearance rate (%)=[1-(E-E0)/(F-F0)] × 100%
In formula:
E:2ml sample liquid adds the absorbance of 2mlDPPH solution;
E0: 2ml water adds the absorbance (sample solvent comparison) of 2mlDPPH solution;
F:2ml sample liquid adds the absorbance (positive control) of 2ml95% ethanol;
F0: 2ml water adds the absorbance (positive control solvent control) of 2ml95% ethanol.
Calculating DPPH clearance rate according to above formula, the more big oxidation resistance of clearance rate is more strong, and experimental result is as shown in table 1.
Table 1
Half suppression ratio (IC50) calculating:
C50Value is defined as the concentration of required antioxidant when clearance rate is 50%. With the active compound A of variable concentrations free radical scavenging being mapped and be fitted, result is Fig. 1 such as, reads and calculates IC50Value. It can be seen that the IC of the DPPH free radical scavenging activity of the active compound of sugary maple liquid50It is 2.8%, there is higher antioxidant activity.
Embodiment two:
A kind of active compound containing sugar maple resin, is made up of by weight following components: sugar maple resin 58 weight portion; Betula platyphylla Suk. myron 25 weight portion; Sucus Cocois 18 weight portion. Three kinds of raw materials are be 800W at microwave power after mixing under 5 DEG C of conditions in temperature, the enzyme denaturing when time is 6min; Mixed liquor after process is 25000rpm at rotating speed after utilizing ice bath to cool to rapidly room temperature, and the time is 14min, and temperature is centrifugal at 3 DEG C, the ultrafilter membrane by 5000Da of the supernatant after centrifugal, obtains permeate; Be 1000rpm, vacuum by liquid in rotary speed being 30Pa, temperature is that under 15 DEG C of conditions, thin film concentration, to the 1/12 of three kinds of raw material mixed liquor initial masses, obtains concentrated solution; It is 40% stabilizer that concentrated solution adds its mass fraction, is the active compound B of the present invention after conventional mixing. Its solid content is 16%-20%, can be directly appended in skin protection cosmetics. Wherein stabilizer is the mixture of propylene glycol, 1,3 butylene glycol, 1,2-pentanediol three, and the mass ratio of mixing is 5:3:2.
Following active compound B is carried out suppresses tyrosinase activity aptitude tests:
In recent years research proves that pigmentation is to be generated enzyme by the melanin in the melanocyte in UV-activated epidermis, caused by chromogenesis. In melanin generation process, tyrosine is changed into DOPA, DOPA quinone by tryrosinase, is polymerized the melanin generating macromole through non-enzymatic oxidation. Therefore by suppressing the activity of tryrosinase can limit melanin generation, the pigmentation of skin is improved.
Sample treatment: the active compound containing sugar maple resin is light yellow transparent liquid, possesses novel aroma, when carrying out tyrosinase inhibition test, is proportionally diluted to desired concn with pure water.
Test method: configuration PBS solution (pH=6.8,0.1mol/L), TYR enzymatic solution (tryrosinase enzyme is lived as 100U/ml). In sample cell and sample controls pipe, each active compound B in 1ml embodiment two, the positive and negative control pipe of adding substitutes with phosphate buffer;Sample cell and sample controls pipe add 0.5ml tyrosinase solution, sample controls and negative control pipe substitute with 0.5ml phosphate buffer, concussion so that sample fully mixes, and hatches 10min for 37 DEG C; Add tryrosinase, after constant temperature 10min, under 475nm, measure its absorbance, and compare with arbutin.
Tyrosinase inhibition rate (%)=[1-(G-G0)/(H-H0)] × 100%
In formula:
G: sample sets;
G0: sample controls group;
H: positive control;
H0: positive solvent control.
Calculating tyrosinase inhibition rate according to above formula, experimental result is as shown in table 2.
Table 2
Half suppression ratio (IC50) calculating:
C50Value is defined as the concentration of required counter inhibitor when suppression ratio is 50%. With the active compound of variable concentrations tyrosinase inhibition rate being mapped and be fitted, result is Fig. 2 such as, reads and calculates IC50Value. It can be seen that the active compound of sugary maple liquid suppresses the IC of tyrosinase activity50It is 4.9%, there is higher suppression tyrosinase activity.
Embodiment three:
A kind of active compound containing sugar maple resin, is made up of by weight following components: sugar maple resin 60 weight portion, Betula platyphylla Suk. myron 30 weight portion, Sucus Cocois 20 weight portion. Three kinds of raw materials are be 900W at microwave power after mixing under 0 DEG C of condition in temperature, the enzyme denaturing when time is 10min; Mixed liquor after process is 18000rpm/min at rotating speed after utilizing ice bath to cool to rapidly room temperature, and the time is 15min, and temperature is centrifugal at 5 DEG C, the ultrafilter membrane by 3000Da of the supernatant after centrifugal, obtains permeate; Be 900rpm, vacuum by liquid in rotary speed being 50Pa, temperature is that under 10 DEG C of conditions, thin film concentration, to the 1/15 of three kinds of raw material mixed liquor initial masses, obtains concentrated solution; It is 30% stabilizer that concentrated solution adds its mass fraction, is the active compound C of the present invention after conventional mixing. Its solid content is 16%-20%, can be directly appended in skin protection cosmetics. Wherein stabilizer is the mixture of propylene glycol, 1,3 butylene glycol, 1,2-pentanediol three, and the mass ratio of mixing is 6:1:2. Carry out respectively active compound C eliminating DPPH free radical aptitude tests and suppressing tyrosinase activity aptitude tests to draw: active compound C has higher antioxidant activity and higher suppression tyrosinase activity.
Embodiment four:
A kind of active compound containing sugar maple resin, is made up of by weight following components: sugar maple resin 55 weight portion, Betula platyphylla Suk. myron 10 weight portion, Sucus Cocois 15 weight portion. Three kinds of raw materials are be 300W at microwave power after mixing under 3 DEG C of conditions in temperature, the enzyme denaturing when time is 5min; Mixed liquor after process is 22000rpm at rotating speed after utilizing ice bath to cool to rapidly room temperature, and the time is 12min, and temperature is centrifugal at 2 DEG C, the ultrafilter membrane by 4000Da of the supernatant after centrifugal, obtains permeate; Be 700rpm, vacuum by liquid in rotary speed being 60Pa, temperature is that under 12 DEG C of conditions, thin film concentration, to the 1/14 of three kinds of raw material mixed liquor initial masses, obtains concentrated solution; It is 20% stabilizer that concentrated solution adds its mass fraction, is the active compound D of the present invention after conventional mixing. Its solid content is 16%-20%, can be directly appended in skin protection cosmetics. Wherein stabilizer is the mixture of propylene glycol, 1,3 butylene glycol, 1,2-pentanediol three, and the mass ratio of mixing is 4:2:1. Carry out respectively active compound D eliminating DPPH free radical aptitude tests and suppressing tyrosinase activity aptitude tests to draw: active compound D has higher antioxidant activity and higher suppression tyrosinase activity.
With specific embodiment, the active compound of the present invention is described further in the application of cosmetics or skin care item below.
Embodiment five:
The active compound A of preparation in embodiment one is added by the present embodiment in the formula of emulsion and prepare emulsion. Wherein the formula of emulsion is as shown in table 3.
Table 3
A phase raw material is mixed, 75 DEG C of dissolvings, and keeps addition B phase at 75 DEG C, stirring, obtain whitening emulsion after cooling.
Embodiment six: in the present embodiment, the active compound B of preparation in embodiment two is added in the formula of astringent and prepare astringent. Wherein the formula of astringent is as shown in table 4.
Table 4
Sequence number |
INCI title |
Add mass fraction/% |
1 |
Sorbitol |
1-3 |
2 |
1,3 butylene glycol |
1.4 |
3 |
PEG1000 |
0.5-1 |
4 |
Brij92 |
1-3 |
5 |
Ethanol |
5-10 |
6 |
Active compound B |
1-40 |
7 |
Essence |
0.01-0.1 |
8 |
Purified Water |
Surplus |
Raw material in above-mentioned table 4 is carried out mixed dissolution, after stirring, obtains astringent.
The following astringent respectively prepared by the emulsion of embodiment five preparation and embodiment six carries out human body white-skinned face function evaluation test.
The active compound used in the present invention, it is possible to as the both effectiveness raw material of whitening and anti-aging cosmetics, its type of service does not have particular/special requirement, and it may be used for water preparation, in the cosmetics of the various different dosage forms such as emulsion. Using the formulation product in embodiment five and embodiment six in the experiment of this application invention human body white-skinned face function, wherein active compound adds mass ratio respectively 10% and 30%.
Tested crowd: be made up of the healthy volunteer in 10 25-45 years.
Subject method: test experimenter makes to apply some make up and is divided into two application area at experimenter's inner forearm marking pen. Experimenter smears given the test agent at inner forearm every day sooner or later, smears blank formula product (without active compound of the present invention) near wrist, uses 28 days continuously. Adopt instrument to gather the melanin value in each region, L-value, and calculate its meansigma methods.
Data acquisition: adopt the MPA580 skinanalysis apparatus of CK company of Germany, wherein MexameterMX18 (melanin and haemachrome test probe) detects dermal melanin, and ColorimeterCL400 (skin color test probe) detects skin complexion uniformity coefficient.
Assessment result: melanin is that we judge the common standard of skin black and white, and the colour of skin gets over brilliant white, and melanin value is more low. As shown in Figure 3, after two test samples use 28 days continuously, the result of sample is smeared in contrast both sides, it is evident that, smear containing active compound 10% and the formulation product melanin minimizing amount containing active compound 30% more than blank, therefore smear the skin protection cosmetics containing active compound 10% and 30% and can generate possess good result to controlling melanin.
L-value is the index defining color, and on skin color, we are used for defining the uniform luminance of the colour of skin. The more uniform brilliant white of the colour of skin, L-value is more high. As can be seen from Figure 4, after two samples use 28 days continuously, that smears that the side L-value of blank sample promotes is less, therefore smears the skin care item containing active compound 10% and 30% or cosmetics and have better effects to promoting skin brightness.
From the above it can be seen that the active compound prepared by the preparation method of the present invention can suppress tyrosinase activity effectively, eliminate free radical, possess good antioxidation; Being applied to prepare cosmetics or skin care item by this active compound, the cosmetics obtained or skin care item, except having natural pure and fresh plant scent, also have lasting antioxidation, whitening effect.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, it is impossible to assert that specific embodiment of the invention is confined to these explanations. For those skilled in the art, without departing from the inventive concept of the premise, it is also possible to make some equivalent replacements or obvious modification, and performance or purposes are identical, all should be considered as belonging to protection scope of the present invention.