The cosmetic use of sal tree seed extract
Technical field
The present invention relates to cosmetic fields, are specifically related to the cosmetic use of sal tree seed extract.
Background technology
Sal tree(Scientific name:Shorea robusta Gaertn.):It is the type sepecies of Shorea.Originate in India and Malaysia
Among the south subtropics rainforest such as peninsula, belong to perennial arbor.Because of its fragrant odour, timber is firm, thus can be used to make furniture or
Building materials, and medicinal or fragrance can be made for.Seed is edible.Resin can be the substitute of pitch, and for coating and make medicinal, natives
It commonly uses to treat the illnesss such as indigestion, leaching disease.It is regarded as one of palo santo by Buddhism.
Sal tree growth is slower.In moist place, it is aithullium, is then machaka in the place of drying,
Almost fall light to its leaf between April in annual February, but grows again to leaf in May.Survival ability
By force.
Modern study discovery, sal seed meal starch-containing 57-60%, protein 10-14%, the also list of 10-14%
Rather.Tannin is added in cosmetics, most direct effect is exactly astriction.Cosmetics containing tannin are under waterproof condition to skin
Skin has good adhesive force, and enlarged pores can be made to shrink, tighten and reduce wrinkle, and skin is made to show fine and smooth appearance.
Sal seed meal is rich in tannin, has very high value to being applied in cosmetics.But at present there has been no
Sal seed and its extract apply the research in cosmetics to report.
Invention content
Present invention aims at sal tree seed extract is provided, using it as the cosmetics of active constituent, its preparation method,
And its application in preparing cosmetics.The present invention specifies that sal tree seed extract has good skin effect and safety
Property, it is a kind of good natural skin care cosmetic raw materials.
In order to realize the above-mentioned purpose of the present invention, the present invention provides the following technical solutions:
A kind of extracting method of sal tree seed extract, includes the following steps:
S1. vacuum microwave pre-processes:Sal tree seed is taken, is crushed, sieving is transferred in vacuum microwave, and it is pre- to carry out vacuum microwave
Processing, obtains pretreatment product;
S2. Extraction solvent is added to step S1 to be made in pretreatment product, refluxing extraction collects extracting solution, and concentrate drying is
Obtain sal tree seed extract.
In wherein some embodiments, grinding mode described in the step S1 include but not limited to grind or shearing or
Ultrasound is preferably ground.
In wherein some embodiments, the sieving described in the step S1 is sieved for 20-40 mesh.
In wherein some embodiments, the pretreated vacuum degree of vacuum microwave described in the step S1 is 0.1-
0.12MPa, microwave treatment time 6-8min, it is 160-180 DEG C to maintain cavity temperature, and microwave treatment dosage is 1.8-2.5kw/
Kg, preferably 2 kw/kg.
In wherein some embodiments, the weight ratio of Extraction solvent and pretreatment product described in the step S2 is(10-
30):1;The Extraction solvent is the ethanol solution of volume fraction 80-90% or the acetone soln of 80-90%, preferably volume point
The ethanol solution of number 90%.
In wherein some embodiments, the number of the refluxing extraction described in the step S2 is 2-4 times, is every time 1-
2h is carried out, preferably 55 DEG C at 50-60 DEG C.
In wherein some embodiments, the step S2 can also make further the extracting solution after obtaining extracting solution
It is refined, for example, by using the methods of ion exchange resin, activated-charcoal column or membrane filtration, preferably membrane filtration.
Wherein, the membrane filtration is preferably smaller than equal to 8000 dongles to be less than or equal to 10000 dalton micro-filtrate membrane filtrations
Pause micro-filtrate membrane filtration, more preferably less than or equal to the micro-filtrate membrane filtration of 5000 dalton.
It, can also be further pure to the extract after the step S2 obtains extract in wherein some embodiments
Change:The purifying purifies, with anhydrous second for 1 part of extract is dissolved into aqueous solution with 100 parts of water through macroporous resin adsorption
Alcohol elutes, concentrate eluant, dry sal tree seed extract.
Inventors be surprised to learn that vacuum microwave processing has larger impact to the efficiency of subsequent extracted, at vacuum microwave
After reason, extraction efficiency is high, few to the tannin component damage of sal tree seed, especially to the yield of the tannin active ingredient of acquisition have compared with
It is big to influence.It is not limited by particular theory, thus it is speculated that it by vacuum microwave the possible reason is handle, due to microwave frequency and change
The whirling vibration frequency for learning group is close, can be used to change the conformation of molecule, selectively activation or brokenization starch and protein
Reactive group promotes chemical reaction, inhibits side reaction, is conducive to promote tannin yield, or is that moisture in cell is quick
Vaporization, forms and acts on cell wall to the vapour pressure of external diffusion, and make breakthroughs in weak links such as pit membranes, cause pit
Film ruptures, to be conducive to subsequent extracted.
The present invention also provides application of the sal tree seed extract in preparing cosmetics.
Further, application of the sal tree seed extract in preparing sun-proof or skin-lightening cosmetic.
Further, application of the sal tree seed extract as cosmetic additive agent in cosmetics, accounting for of additive amount
The 0.01-1wt% of cosmetic gross mass.
Further, the cosmetics can be facial treatment milk.
Further, facial treatment milk includes the component of following mass percentage, as shown in table 1:
Table 1
Compared with prior art, the present invention has following advantageous effect:
The present invention obtains Objective extraction object by being extracted to sal tree seed, and cytotoxicity experiment has been carried out to Objective extraction object
With sun-proof experiment, it was demonstrated that the safety of Objective extraction object and the absorbability of ultraviolet light specify that Objective extraction object is excellent
Cosmetic active and pharmaceutical activity.The present invention improves the utilization function and added value of sal tree seed, and has expanded natural skin care
The source of product plant material.The present invention provides a kind of sal tree seed extracting methods, including:Sal tree powder of seeds is subjected to vacuum
It is extracted after Microwave Pretreatment, obtains extract, the extracting method extraction efficiency is high, does not introduce to human body harm excitatory
Object destroys the tannin of sal tree seed sal tree seed extract tannin content and the purity height few, which extracts, helps
In the performance of sal tree seed effect, also, the extracting method is easily operated, is suitable for industrialization promotion application.Experimental result is demonstrate,proved
Bright, the sal tree seed extract high safety of extracting method extraction has notable sun-proof, whitening effect.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, embodiment of the present invention will be made into one below
Step ground detailed description, embodiments of the present invention are not limited thereto, for not specifically specified technological parameter or condition, can refer to
Routine techniques carries out.
Embodiment 1
The preparation of sal tree seed extract:
S1. net sal tree seed 100g is weighed, is smashed, the sieving of 20 mesh is transferred in vacuum microwave, it is pre- to carry out vacuum microwave
Processing, holding vacuum degree are 0.1MPa, microwave dose 1.8kw/kg, processing time 6min, and it is 160 to maintain microwave cavity temperature
DEG C, obtain pretreatment product;
S2. after the pretreatment of S1 step vacuum microwaves, pre- place is added to the ethanol solution of the volume fraction 80% of 10 times of weight
It manages in product, 50 DEG C of refluxing extraction 1h are repeated 2 times, and collect extracting solution, concentration, and 50 DEG C of dryings obtain sal tree seed extract
12.2g, recovery rate 12.2%.
Embodiment 2
The preparation of sal tree seed extract:
S1. net sal tree seed 100g is weighed, is smashed, the sieving of 40 mesh is transferred in vacuum microwave, it is pre- to carry out vacuum microwave
Processing, holding vacuum degree are 0.12MPa, microwave dose 2.5kw/kg, processing time 8min, and maintenance microwave cavity temperature is
180 DEG C, obtain pretreatment product;
S2. after the pretreatment of S1 step vacuum microwaves, pre- place is added to the ethanol solution of the volume fraction 90% of 30 times of weight
It manages in product, 60 DEG C of refluxing extraction 2h are repeated 4 times, and are collected extracting solution and are obtained refined filter using 10000 dalton micro-filtrate membrane filtrations
Refined filtrate is evaporated under reduced pressure by liquid with Rotary Evaporators, concentration, 60 DEG C of dryings obtain crude extract, and 1 part is carried with 100 parts of water
It takes object to be dissolved into aqueous solution, is purified through macroporous resin adsorption, then with anhydrous ethanol elution, collect eluent concentration, cryogenic freezing
Drying is to get sal tree seed extract 14g, recovery rate 14%.
Embodiment 3
The preparation of sal tree seed extract:
S1. net sal tree seed 100g, Ultrasonic Pulverization are weighed, the sieving of 30 mesh is transferred in vacuum microwave, it is pre- to carry out vacuum microwave
Processing, holding vacuum degree are 0.11MPa, microwave dose 2kw/kg, processing time 7min, and it is 170 to maintain microwave cavity temperature
DEG C, obtain pretreatment product;
S2. after the pretreatment of S1 step vacuum microwaves, pre- place is added to the acetone soln of the volume fraction 85% of 20 times of weight
It manages in product, 55 DEG C of refluxing extraction 1.5h are repeated 3 times, and are collected extracting solution and are obtained refined using 5000 dalton micro-filtrate membrane filtrations
Refined filtrate is evaporated under reduced pressure by filtrate with Rotary Evaporators, and concentration, 55 DEG C of dryings obtain crude extract, with 50 parts of water 1 part
Extract is dissolved into aqueous solution, is purified through macroporous resin adsorption, then with anhydrous ethanol elution, collects eluent concentration, low temperature cold
It is lyophilized dry to get sal tree seed extract 13.8g, recovery rate 13.8%.
Comparative example 1
Without vacuum microwave pre-treatment step S1, remaining step and condition are the same as embodiment 1.
Obtain sal tree seed extract 4.8g, recovery rate 4.8%.
Comparative example 2
Without vacuum microwave pre-treatment step S1, remaining step and condition are the same as embodiment 2.
Obtain sal tree seed extract 5.4g, recovery rate 5.4%.
Comparative example 3
Without vacuum microwave pre-treatment step S1, remaining step and condition are the same as embodiment 3.
Obtain sal tree seed extract 5.2g, recovery rate 5.2%.
Embodiment 4:The sal tree seed extract of embodiment 1-3 and comparative example 1-3 is added separately in following formulas,
Facial treatment milk is made, is calculated as facial treatment milk 1-6 successively, wherein facial treatment milk 1-6 includes each group of following mass percentage
Point, as shown in table 2:
Table 2
Efficacy test of the present invention:
1, tannin content detects
Present invention combination standard GB/T/T 15686-2008, utilizes tannin and Fe3+It can the stable purple of fast reaction generation
The property of red complex establishes a kind of rapid detection method can be applied to tannin content in extract.And with embodiment
The sal tree seed extract of 1-3 and comparative example 1-3 is detection sample, is detected to its tannin content.
1)Testing principle
Tannin reacts under weakly alkaline environment with iron ion, generates aubergine complex, the depth of this complex compound color
It is directly proportional to the size of tannin content in sample.Its absorbance value is measured at 525 nm wavelength with spectrophotometer, with standard
Series of comparisons is quantified.
2)Test method
The drafting of tannin standard curve:Using tannic acid as standard items, it is diluted to 0 with 75% dimethyl formamide solution,
0.001,0.01,0.1,0.2,0.3,0.4,0.5,1.0 g/mL standard serial solutions pipette 1mL in test tube, successively respectively
Accurate that 5 mL water, 1mL3.5g/L ironic citrates ammonium salt solution, 1mL8.0 g/L ammonia solutions is added, oscillation shakes up, and room temperature is protected from light standing
10 min.Be poured into cuvette, with spectrophotometer in wavelength be at 525n measurement absorbance value.Made simultaneously with water empty
In vain.
Specimen Determination:Extract sample preparation is at 0.1,0.2,0.5,1.0,2.0,5.0g/L standard serial solution, respectively
The accurate extract solution 1mL that draws sequentially adds 6mL distilled water and the ammonia solution of 1mL8.0g/L, vibrates in the 1st batch of test tube
It shakes up, blank is made with water after 10 min, with spectrophotometer in the absorbance value that wavelength is measurement sample solution at 525 nm
A1.Accurate 1 mL extracting solutions of drawing sequentially add 5 mL water, 1mL3.5g/L ferric citrates in the 2nd batch of test tube respectively
Solution vibrates, then adds 1mL8.0g/L ammonia solutions, and oscillation shakes up rear timing,(10±1)After min, blank is made with water, is surveyed in 525nm
Determine the absorbance value A of sample solution2.The absorbance measurement result A=A of tannin in sample2-A1, sample is gone out by regression equation calculation
The mass concentration c of product solution tannin.Tannin content indicates with the mass fraction of tannic acid in butt, i.e. the c of tannin content=2
1000/m.In formula, c is the mass concentration of the tannin checked in from standard curve(mg/mL);M is sample quality(g).
Tannin content in the different sal tree seed extracts of table 3
As can be known from the above table, the tannin content of the sal tree seed extract obtained by 1-3 of the embodiment of the present invention is relative to comparative example 1-3 high
In 200%(920.2/323.8*100% > 200%).It can be seen that the present invention is after vacuum microwave pre-processes, then through ethyl alcohol
Or in the obtained sal tree seed extract of acetone extraction tannin content and purity all highers, vacuum microwave pretreatment is key step
Suddenly, there is larger impact in the step for the yield of tannin, and after this pretreatment, to Extraction solvent such as ethyl alcohol, acetone
Concentration requirement reduces.
2, the cytotoxicity experiment of sal tree seed extract:By MTS colorimetric methods, the CC of sample is determined50(50%
Cytotoxicconcentration), i.e., drug concentration when generating toxicity to 50% cell, so that it is determined that following activity is real
The secure sample concentration tested.
Experimental method:In 96 porocyte culture plates, B16 cells are mixed with the drug solution to be measured of various concentration, setting 3
A repeating hole, while the blank control of not drug containing is set, 37 DEG C, 5%CO2It cultivates for 24 hours, using MTS colorimetric determination cells
Toxicity, microplate reader measure OD values, measure wavelength 490nm.CC is calculated50Value.
Cell survival rate (%)=experimental port OD490nm/ blank well OD490nm× 100%
Experimental result:The cell survival rate of sal tree seed extract is respectively 89.35%, 88.76% obtained by embodiment 1-3,
88.96%,:Equal > 60% belongs to normal level, it is evident that sal tree seed extract does not have toxic action to cell, as
The safety of the natural material of cosmetics for skin is guaranteed.
3, sun-proof test:
Ultraviolet light (UV) included in sunlight is the wavelength light shorter than the wavelength of the visible light of human-perceivable.It can reach in ground
The ingredient of the UV of table be divided into the UV-A (long wavelength UV) that wavelength is 320-400nm and the UV-B that wavelength is 290-320nm (in
Wavelength UV).The radiation of these UV can allow skin to generate a large amount of free radicals, lead to the peroxidization of cell membrane, make melanin
Cell generates more melanin, and is up distributed to horny layer of epidermis, causes black splotch.Ultraviolet light can be described as causing skin
Skin wrinkle, aging, relaxation and blackspot maximum arch-criminal.
Experimental animal:The mouse 35, weight 180-220g for taking health, is randomly divided into 7 groups, every group of 5 mouse:One group is sky
White group, 6 groups are experimental group (1% concentration of aqueous solution of sal tree seed extract for smearing embodiment 1-3 and comparative example 1-3 respectively).
Experimental method:Each group mouse carries out back depilation with the sodium sulphate of 0 .8%, leaks the test section of 6cm × 6cm cruelly.
Skin first is cleaned with warm water before smearing sample, the mouse for being coated with given the test agent solution is placed on 1h in sunlight simulated experiment case,
It is carried out continuously 3 months, during which shaves off the mouse hair newly grown in time.Finally, test mice skin is tested using dermal melanin instrument
Melanin content MI values, experimental result are shown in Table 4:
Can be seen that embodiment 1-3 and comparative example 1-3 from upper table data can reduce melanin MI values, and 1-3 of the embodiment of the present invention
Sal tree seed extract sun-proof result is more notable, can be used in sun-proof or whitening class cosmetics.
6, crowd's test on probation
For the practical effect of test product, crowd's investigation on probation, group have been carried out respectively to sample made from facial treatment milk 1-6
Send out volunteer of the sample to 300 ages 26-40 Sui(Wherein women 238), health, rule of life, no skin disease,
Volunteer is divided into 6 groups at random.After volunteer cleans facial skin, dries, appropriate facial treatment milk is applied to left side of the face with hand
Portion, right side face does not smear, and as test comparison area, tested period face does not smear other cosmetics or drug, continuously makes
Using effect was checked with 30 days, and filled in questionnaire.
It is classified the standard of judgement:
Significantly effectively:Opposite right side face, test block color spot problem are completely resolved, and skin smooth is for example new, the white and moist pool of jade-like stone, skin
Skin high resilience.
Effectively:Opposite right side face, test block color spot is obviously thin out, forms color spot soon or even can completely disappear, skin
Skin becomes pale, and skin becomes flexible.
In vain:Opposite right side face, test block color spot do not change without significant change or intensification, the colour of skin.
Crowd tries out investigation result table 5
Conclusion:In the facial treatment milk sample of the seed extract containing sal tree, facial treatment milk 1-3 of the present invention, after using 30 days, skin
Skin is smooth as new, and the white and moist pool of jade-like stone, skin becomes flexible.And it adds and lacks the sal tree seed that vacuum microwave pre-treatment step obtains
The facial treatment milk 4-6 of extract, after using 30 days, skin improves situation(It is significantly efficient≤9)It can not show a candle to facial treatment milk
The effect of 1-3(It is significantly efficient >=42).Illustrate that facial treatment milk of the present invention has good whitening effect.
It is learnt through questionnaire, using facial treatment milk product of the present invention, mild non-stimulated, skin sense is fine.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to the model of the present invention
It encloses and is defined, under the premise of not departing from design spirit of the present invention, technical side of the those of ordinary skill in the art to the present invention
The various modifications and improvement that case is made should all be fallen into the protection domain of claims of the present invention determination.