CN105726343A - Preparing method of small water molecular clusters TMW for improving cosmetic activity - Google Patents
Preparing method of small water molecular clusters TMW for improving cosmetic activity Download PDFInfo
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- CN105726343A CN105726343A CN201610100851.2A CN201610100851A CN105726343A CN 105726343 A CN105726343 A CN 105726343A CN 201610100851 A CN201610100851 A CN 201610100851A CN 105726343 A CN105726343 A CN 105726343A
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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
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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Abstract
The invention relates to a preparing method of small water molecular clusters TMW for improving cosmetic activity. The preparing method includes the following steps that 1, liquid water is frozen to prepare ice; 2, in vacuum, the ice is sputtered with lasers to generate plasma containing the small water molecular clusters TMW. The small water molecular clusters TMW prepared through the method are high in activity, and cosmetic activity can be improved.
Description
Technical field
The present invention relates to cosmetic field, more particularly it relates to an promote the small water molecule cluster of cosmetic activeTMWPreparation method.
Background technology
Hydrone contains an oxygen atom and two hydrogen atoms, aqueous water and solid water do not only exist the covalent bond between hydrogen atom and oxygen atom in molecule, and there is intermolecular interaction, this intermolecular interaction is the hydrogen bond formed with the oxygen atom in another one hydrone by the hydrogen atom in a hydrone, and this intermolecular force is also called Van der Waals force.In aqueous water, it is common that got up by hydrogen bonded with several hydrones；But in solid water, namely inside ice, hydrone interconnects with hydrogen bond in a wider context, form the crystal of loose rule.X ray research shows, ice has tetrahedral crystal structure, and this tetrahedral lattice is that five hydrones are formed by intermolecular hydrogen bonding, and crystals arrangement in order, has fixing space.After ice-out Cheng Shui, break the hydrogen bond of a large amount of rule and regular crystal structure, made tetrahedral lattice be structured as scattered molecular radical, so aqueous water no longer ordered arrangement as ice, but define unordered structure.
Research shows, after forming small water molecule cluster by hydrogen bond between hydrone, dissolving power, penetration, metabolism power and emulsifying capacity all strengthen to some extent, thus having certain activation.Cosmetics use small water molecule cluster can improve the activity of cosmetics.At present, traditional prepares small water molecule cluster (TMW, the abbreviation of TinyMolecularWater) adopt electromagnetic method, Mechanical Method, supercritical ultrasonics technology, far infrared collimation method, function ceramics method, information model method etc. more, small water molecule liveness prepared by these methods is low, and prepared by the multiplex aqueous water of these methods, produced small water molecule is unordered chaotic structure, not only can not improve the activity of small water molecule itself, can not be used for promoting the activity of cosmetics.
Therefore it is highly desirable to a kind of method that can prepare high activity and regular small water molecule cluster, enables small water molecule cluster to promote the activity of cosmetics.
Summary of the invention
For solving above-mentioned technical problem, the preparation method that the present invention provides a kind of small water molecule cluster (TMW) promoting cosmetic active, described small water molecule cluster (TMW) has significantly high activity, it is possible to be used for promoting the activity of cosmetics.
The preparation method that one aspect of the present invention relates to a kind of small water molecule cluster (TMW) promoting cosmetic active, comprises the steps of
(1) ice is prepared in aqueous water freezing；
(2) under vacuum, utilizing laser splash ice, produce small water molecule cluster (TMW), described small water molecule cluster (TMW) is plasma state.
In one embodiment, in the preparation method of a kind of small water molecule cluster (TMW) promoting cosmetic active of the present invention, one or more in following material of aqueous water in described step (1): distilled water, deionized water, mineral water, tap water.
In one embodiment, in the preparation method of a kind of small water molecule cluster (TMW) promoting cosmetic active of the present invention, in described step (1), aqueous water is deionized water.
In one embodiment, in the preparation method of a kind of small water molecule cluster (TMW) promoting cosmetic active of the present invention, described mineral water comprises one or more in following metallic element: ferrum, potassium, magnesium, aluminum, zinc, silver, sodium, titanium.
In one embodiment, in the preparation method of a kind of small water molecule cluster (TMW) promoting cosmetic active of the present invention, in described step (2), the vacuum of vacuum condition is 2 × 10-1Pa～8 × 10-3Pa。
In one embodiment, in the preparation method of a kind of small water molecule cluster (TMW) promoting cosmetic active of the present invention, in described step (2), the optical maser wavelength for sputtering is the one in 266nm, 355nm, 532nm, 1064nm.
In one embodiment, in the preparation method of a kind of small water molecule cluster (TMW) promoting cosmetic active of the present invention, the described optical maser wavelength for sputtering is 1064nm.
In one embodiment, in the preparation method of a kind of small water molecule cluster (TMW) promoting cosmetic active of the present invention, the described laser energy for sputtering is 10～50mJ.
Another aspect of the present invention relates to a kind of cosmetics, the small water molecule cluster (TMW) that described toiletry bag is prepared containing method of the present invention.
The preparation method that another aspect of the present invention relates to a kind of cosmetics, comprise the steps of and cosmetics are placed in magnetic field, under being stirred continuously, the small water molecule cluster (TMW) preparation method of small water molecule cluster of the present invention (TMW) obtained deposits in cosmetics.
In one embodiment, in the preparation method of a kind of cosmetics of the present invention, the magnetic induction in described magnetic field is 0.003～0.8T, and frequency is 5～50kHz.
It is more readily understood the above-mentioned of the application and other features, aspect and advantage with reference to described further below.
Accompanying drawing explanation
Small water molecule cluster (TMW) and the schematic diagram containing small water molecule cluster (TMW) cosmetics are prepared in Fig. 1 expression.
The wherein explanation of accompanying drawing labelling:
1-noble gas；2-valve；3-stainless steel pipes；4-quartz glass window；5-laser；6-reative cell；7-sample cell；8-liquid nitrogen；9-stainless steel pipes；10-agitator；11-receiving chamber；12-magnetic field.
Detailed description of the invention
Detailed description and embodiment with reference to the specific embodiment of the present invention can be more easily understood present disclosure.Being described below in book and claims and can mention a large amount of term, these terms are defined as following implication.
In present specification and claims, scope limits and can combine and/or exchange, and without other explanation, these scopes include all subranges contained therebetween.Word " comprise " be not intended to get rid of other, additive, component, integer or step.Approximate term in specification and claims is used for modifying quantity, represents that the present invention is not limited to this particular number, also includes close to this quantity acceptable without causing the part of the correction of the change of relevant basic function.In some example, approximate term likely corresponds to measure the precision of the instrument of numerical value.
In the present invention, described term " TMW " refers to the English explanation of small water molecule cluster.
The preparation method that the first aspect of the invention relates to a kind of small water molecule cluster (TMW) promoting cosmetic active, it is characterised in that comprise the steps of
(1) ice is prepared in aqueous water freezing；
(2) under vacuum, utilizing laser splash ice, produce small water molecule cluster (TMW), described small water molecule cluster (TMW) is plasma state.
First aqueous water is frozen into ice.Then, as it is shown in figure 1, in the sample cell 7 being placed in by ice in reative cell 6, sample cell 7 liquid nitrogen 8 freezes, and maintains the temperature at less than-75 DEG C, evacuation；The upside of reative cell 6 is provided with quartz glass window 4, transparency range can reach 200nm, laser 5 light beam is made to be irradiated to ice surface by quartz glass window 4, laser splash can produce small water molecule cluster (TMW), small water molecule cluster (TMW) is plasmoid, in sputter procedure, regulate laser optical path every 10min, change laser spot position.
Described sputtering refers to bombards the surface of solids with the particle (ion, photon or neutral atom, molecule) of certain energy, makes the atom on the nearly surface of solid or molecule obtain sufficiently large energy and the surface of solids of finally overflowing.Sputtering can only carry out under certain vacuum state.
Water is cosmetics and the indispensable material of skin, the method utilizing pulsed laser deposition, by height collimation, high-octane pulse laser focusing on ice crystal, in ice crystal, hydrone absorbs pulsed laser energy, produce plasma, plasma includes small water molecule cluster and the electronics of cation, anion and neutrality；Further, after portion of water absorbs pulsed laser energy, Electron absorption energy on the molecular orbit of water, from ground state transition to excited state, form the small water molecule cluster (TMW) of excited state.The small water molecule cluster activity that this method produces is higher, and size distribution is uniform.In ice, each hydrone forms the ordered arrangement of orientation by hydrogen bond, when ice melts naturally as aqueous water, a large amount of hydrogen bonds are broken, ice crystal turns to the aqueous water of lack of alignment, distance between hydrone changes, unlike in ice crystal fixing, some hydrone can enter in other lattice.In the present invention, using superlaser to be splashed to the surface of ice, directly produce small water molecule cluster plasma, formed small water molecule cluster size is more uniform.
Use aqueous water of the present invention prepares into the step of ice can adopt various technology well known by persons skilled in the art, for instance slice ice machine, plate ice machine, tube ice machine, shell ice machine, granule ice maker etc..
In one embodiment, in the preparation method of a kind of small water molecule cluster (TMW) promoting cosmetic active of the present invention, one or more in following material of aqueous water in described step (1): distilled water, deionized water, mineral water, tap water.
The distilled water that the present invention adopts meets " Pharmacopoeia of People's Republic of China (2000 editions) " purified water " " standard.Distilled water for the present invention can use method known to those skilled in the art to prepare, such as distillation machine etc..It is also commercially available for may be used for the distilled water of the present invention.
In one embodiment, it is preferable that in the preparation method of a kind of small water molecule cluster (TMW) promoting cosmetic active of the present invention, in described step (1), aqueous water is deionized water.Deionized water is complete or removes the water of ionic species by halves.Use small water molecule cluster (TMW) purity that deionized water is formed high, the plasma formed will not be subject to the harmful effect of other impurity.
Deionized water for the present invention can be commercially available, meets International Organization for Standardization ISO/TC147 regulation.
In one embodiment, in the preparation method of a kind of small water molecule cluster (TMW) promoting cosmetic active of the present invention, described mineral water comprises one or more in following metallic element: ferrum, potassium, magnesium, aluminum, zinc, silver, sodium, titanium.
Mineral element in described mineral water, skin is favourable, through high energy pulse laser splash, mineral element can obtain or lose a mineral ion electronically forming gaseous state, and form ion cluster with the hydrone of surrounding, each metal ion can in conjunction with the hydrone of more than 1, wherein, portion of water is by H atom or oxygen atom and metal center coordination, forming endothecium structure, other hydrone is connected with the hydrone of internal layer by the effect of hydrogen bond, forms layer structure.The mineral element of such trace can with the form of ionic state close to skin, and by the affinity interaction of electrostatic attraction and hydrone and phospholipid bilayer by percutaneous absorption.The hydrophilic group of the phospholipid bilayer of surface of cell membrane is outside, and with certain electric charge, the metal ion of water molecule coordination enters cell interior more easily by cell membrane.
Mineral water for the present invention adopts technology well known by persons skilled in the art to prepare, for instance with city tap-water for former water, processes then through purification, adds mineral, obtain mineral water after sterilization processing.The mineral of the trace added is for can improve cosmetic active, the mineral element of strengthening skin regeneration function, can need to choose according to cosmetics, for instance abundant calcium and magnesium have skin of releiving, increasing the effect of elasticity of skin and toughness, silver element has antibacterial and antioxidative effect etc..
For the tap water of the present invention from waterworks, meeting " country's Drinking Water related sanitary standard ", the microbiological indicator of described tap water, toxicological parameters, sensory properties and general chemical index, radioactive indicator etc. all meet national standard.
In one embodiment, in the preparation method of a kind of small water molecule cluster (TMW) promoting cosmetic active of the present invention, in described step (2), the vacuum of vacuum condition is 2 × 10-1Pa～8 × 10-3Pa。
In one embodiment, it is preferable that in the preparation method of a kind of small water molecule cluster (TMW) promoting cosmetic active of the present invention, in described step (2), the vacuum of vacuum condition is 2 × 10-2Pa。
It is commercially available mechanical pump and molecular pump for producing the vacuum equipment of the present invention.Described mechanical pump is mechanically bleed and obtain the equipment of vacuum being taken out container, and the one in reciprocating machine pump, stator formula mechanical pump and rotary vane mechanical pump, the ultimate pressure that can reach is 1Pa～0.01Pa.Described molecular pump be the rotor utilizing high speed rotating MOMENTUM TRANSMISSION to gas molecule, so as to obtain directed velocity, thus a kind of vacuum pump taken away for prime after being compressed, being driven to air vent, limiting pressure is up to 10-9Pa.Preferably, it is turbomolecular pump for the molecular pump of the present invention.Described molecular pump need to be equipped with the mechanical pump as backing pump and use.
In one embodiment, in the preparation method of a kind of small water molecule cluster (TMW) promoting cosmetic active of the present invention, in described step (2), the optical maser wavelength for sputtering is the one in 266nm, 355nm, 532nm, 1064nm.
Laser instrument for the present invention has no particular limits, it is possible to be the one in gas laser, solid state laser, liquid laser, semiconductor laser and free electron laser.
In one embodiment, in the preparation method of a kind of small water molecule cluster (TMW) promoting cosmetic active of the present invention, preferably, described laser instrument is Nd:YAG laser instrument, described laser instrument is made up of operation material, pumping source resonant cavity three part, and operation material is mixed with a certain amount of neodymium ion (Nd3+) yttrium-aluminium-garnet (YAG) crystal.The wavelength of the laser that described Nd:YAG laser instrument can export includes 266nm, 355nm, 1064nm, 532nm；Laser energy is 10～800mJ, and beam diameter is 8mm, and beam divergence angle < 0.8, pulse width 1～20ns.
In one embodiment, in the preparation method of a kind of small water molecule cluster (TMW) promoting cosmetic active of the present invention, it is further preferred that the optical maser wavelength that the Nd:YAG laser instrument used in method of the present invention produces is 1064nm, laser energy is 10～50mJ.
The different material laser to different wave length, and the laser absorption of different-energy has selectivity, in order to make the water molecule cluster of laser splash have suitable size, and the hydrone controlling excited state absorbs the photon energy of specific wavelength, make at energy after intermolecular transfer, play optimum efficiency to promoting cosmetic active, the wavelength of laser instrument, energy density need to be adjusted.On the other hand, the absorption of the light of different wave length is also had selectivity by human body different tissues, different through the cosmetic active of different laser treatment, can be also different by the energy of skin histology selective absorbing, for effectively solving skin problem, promote skin metabolism, inventor have found that the cosmetic effect through the above-mentioned laser conditions of overtesting discovery is obtained is splendid.
In one embodiment, in the preparation method of a kind of small water molecule cluster (TMW) promoting cosmetic active of the present invention, it is more preferable to ground, the described laser energy for sputtering is 20mJ.
At beam diameter, beam divergence angle, pulse width, when other parameter constants such as optical maser wavelength, when as required laser energy being adjusted, the energy affect laser splash of laser to aqueous water surface and internal time, the energy density of laser and sputter temperature, and the size of the small water molecule cluster finally produced, cluster institute is electrically charged, cluster institute band energy, the electronic state of excited state, so the small water molecule cluster of different activities can be produced, and then the raising degree that impact is to cosmetic active, the present inventor finds through experiment, when laser energy is 20mJ, the gained small water molecule cluster (TMW) the lifting best results to cosmetic active.
A second aspect of the present invention relates to a kind of cosmetics, the small water molecule cluster (TMW) that described toiletry bag is prepared containing method of the present invention.
Described cosmetics can be the cosmetics of various form well known by persons skilled in the art, comprises and be not limited to water preparation, emulsion, facial cream, eye cream, facial milk cleanser, facial film, BB liquid white, consummate, sunscreen cream, sun water, acne water, lotion for pimples, face cleaning water, face cleaning dew, quintessence oil, shampoo.Described water preparation is transparent liquid class cosmetics, comprises and be not limited to moisture retention water, cosmetic water, astringent lotion, toner/smoothing toner.Described emulsion, facial cream are liquid frost class cosmetics.Described facial milk cleanser, face cleaning water, face cleaning dew refers generally to the liquiform product being made up of compositions such as oil phase thing, aqueous-phase material, surfactant, wetting agent, nutrients, includes but not limited to cleansing milk, facial cleaning cream, clean skin liquid.Described facial film is a kind of carrier of face beautifying health keeping product, includes but not limited to mud cream type, tear-pull, gel-type, wet paper towel profile film.Described BB frost refers to that BlemishBalm, effect include but not limited to hide the flaw, adjust the colour of skin, pore sun-proof, careful.Described consummate liquid refers to comprise the high nutrient of concentration, includes but not limited to the forms such as essence, elite dew, elite facial film, essence injection, " Jinghuasu " essence capsule.Described sunscreen cream is with the addition of to intercept or absorb ultraviolet sunscreen and reach to prevent skin by cosmetics tanned, sunburn.Described acne water is the liquid with treatment acne effect.Described lotion for pimples is the liquid with treatment acne function.Described quintessence oil is from the flower of plant, leaf, stem, root or fruit, is refined the volatile flavor extracted by steam distillation, squeezing and pressing method, cold-maceration or solvent extraction method.Described shampoo is cleaning and the goods of maintenance hair and skin.
The preparation method that a third aspect of the present invention relates to a kind of cosmetics, comprise the steps of and cosmetics are placed in magnetic field, under being stirred continuously, the small water molecule cluster (TMW) preparation method of small water molecule cluster of the present invention (TMW) obtained deposits in cosmetics.
After described deposition refers to the place that the material that passive movement medium is carried reaches to be suitable for, the effect of the process precipitate owing to condition changes, piled up.
As shown in Figure 1, after producing small water molecule cluster plasma, open the valve 2 on stainless steel pipes 3, in reative cell 6, noble gas 1 is passed into by stainless steel pipes 3, noble gas 1 has the movement velocity of orientation, and carrier band small water molecule cluster forms plasma molecular beam, various particles within molecular beam do high-speed motion, the introducing of intert-gas atoms, the internal collision cooling that appropriateness occurs of molecular beam can be made, in above laser splash process, portion of water is broken up the atom or atomic group that become separation by high energy laser 5, atom or atomic group are ionized to as negative ions, collision cooling makes them recombine becomes highly active small water molecule cluster, molecular beam moves along the direction of noble gas, enter in receiving chamber 11 through second stainless steel pipes 9, deposit in cosmetics.Receiving chamber is in the magnetic field 12 with some strength, and uses agitator 10 to be stirred continuously cosmetics, utilizes magnetization technology to mix with small water molecule cluster in cosmetics, and whole flow process is different according to cosmetics consumption, and the persistent period is different.
Described noble gas one in helium, argon.
In magnetic field, in polar water molecules and cosmetics, the molecular motion track of active component is constantly twisted, in hydrone and cosmetics, the more weak effect between active ingredient molecule is interrupted, and stronger active force preserves, and forms the cosmetic actives molecules surrounded by small water molecule cluster.Finally, small water molecule cluster (TMW) connects together with active group contained in cosmetics, this connection includes covalent bond, hydrogen bond, Van der Waals force, electrostatic attraction, it is partially in the molecule of excited state through relaxation process, realize the transmission of intermolecular energy, the effective ingredient contained in cosmetics is made to be in low-lying excitation state, but the molecular moiety being wherein in the effective ingredient of low-lying excitation state can with positive charge, part can with negative charge, and the cosmetics of entirety belong to neutral substance, in cosmetics useful life, it is in steady statue.
Described relaxation process refers to that a macroscopic equilibrium system due to the change of surrounding or is subject to the effect in the external world and becomes nonequilibrium condition, and this system is transitioned into the process of new equilibrium state again from nonequilibrium condition.In relaxation process substantially system microcosmic particle due to interaction positive energy exchange, finally reach the process of Stable distritation.
Skin is divided into epidermis, corium and subcutaneous tissue three part, and epidermis ground skin plays barrier action；Corium is the essence of skin, and epidermis completes skin function jointly；Corium and epidermis are played supporting role by subcutaneous tissue.Generally, the cosmetics of use work just for epidermis, and skin is played barrier action by epidermis, and epidermal structure is divided into again five layers, are horny layer, clear layer, granular layer respectively, have spinous layer, basal layer.The water content of keratodermatitis is in certain limit, skin just can smooth, soft and high resilience, keep skin to be in good state, it is considered that in the best state more than 10%, be easy for lower than 10% drying, coarse.Intercellular lipid has obvious bilayer structure, and namely lipophilic group is inside, and hydrophilic group is outside, forms the sandwich structure that water fat is alternate, and cell membrane is also made up of the phospholipid bilayer being inlaid with protein, and with certain electric charge.This structure makes biomembrane have the half penetrating character with selective permeation, the absorption being conducive to some little molecular nutrition material is permeated, on the other hand, it combines portion of water and the latter is fixed up, these hydrones are exactly so-called Bound moisture, even if without loss when very dry.Moisture of skin is lost, and can cause xerosis cutis, desquamation etc..The exception of lipid barrier can reduce the moisture preserving function of skin, and the growth also directly affecting corneocyte regulates with differentiation, and unhealthful horny layer is formed.
After the small water molecule cluster (TMW) method of the present invention prepared mixes in magnetic field with cosmetics, in cosmetics, bioactive molecule is surrounded by the small water molecule cluster (TMW) of activity on the one hand, higher with the hydrophilic group affinity of phospholipid bilayer, and it is higher with the electrostatic interaction of the phospholipid bilayer with certain electric charge, on the other hand also in low-lying excitation state, improve the skin absorption efficiency to the cosmetic active factor and the content of the Bound moisture of epidermis.
For producing the device in magnetic field required for the present invention, there is no particular limitation, it is possible to is commercially available magnetic field generator, it is also possible to is by alternating current passes into the magnetic field that solenoid is formed.Acting as of magnetic field utilizes magnetic field to make cosmetics mix with small water molecule cluster (TMW).
Stirring means for the present invention is mechanical agitation, the agitator adopted is agitator well known by persons skilled in the art, for instance flat paddle agitator, propeller stirrer, turbine type agitator, anchor agitator, squirrel-cage agitator, planet strrier etc..
In one embodiment, in the preparation method of a kind of cosmetics of the present invention, the magnetic induction in described magnetic field is 0.003～0.8T, and frequency is 5～50kHz.
In one embodiment, it is preferable that, in the preparation method of a kind of cosmetics of the present invention, the magnetic induction in described magnetic field is 0.05T, and frequency is 20kHz.
Being placed in magnetic field by cosmetics, magnetic field can affect moving direction and the speed of bioactive molecule and small water molecule cluster in cosmetics, and affects intermolecular energy transfer process, the activity of the gained cosmetics of final impact.On the other hand, magnetic field and electric field can be changed mutually, and the cell membrane of antibacterial receives the effect of strong electric field can produce violent concussion, and antibacterial can be pulverized by the plasticity scope beyond cell membrane, so the effect of sterilization can be played.The inventors discovered that, when the magnetic induction in magnetic field is 0.05T, when frequency is 20kHz, gained cosmetic active is best.
By the examples below the present invention is specifically described.Be necessary it is pointed out here that be; following example are served only for that the invention will be further described; it is not intended that limiting the scope of the invention; some nonessential improvement and adjustment that professional and technical personnel in the field makes according to the content of the invention described above, still fall within protection scope of the present invention.
The equipment used and sample:
Mechanical pump: twin-stage high speed direct connection structure sheet vacuum pump, buys from Beijing Midwest Co., and model is 2XZ-4B.
Molecular pump: turbomolecular pump, buys from thing instrument (Beijing) Science and Technology Ltd., and model is F-100/110.
Laser instrument: Nd:YAG laser instrument is bought from Han Yu Science and Technology Ltd., and model is LPY600/700.
Magnetic field generator: buy and exchange high-intensity magnetic field generation systems from Qingdao Zhong Yuhuantai magnetoelectricity Science and Technology Ltd..
Agitator: buy from VELP company of Italy, DLH overhead type stirrer.
Not aqueous cosmetics emulsion: choose following for preparing the usual ingredients of emulsion, by weight: microcrystalline wax 1, Cera Flava 2, lanoline 2, liquid paraffin 20, isotriacontane 10, Span-83 4, polyoxyethylene (20) sorbitan monooleate 1, propylene glycol 7.The technology adopting conventional homogenizer prepares into not aqueous emulsion.
Deionized water；Tap water；Mineral water containing, for example lower metallic element: ferrum, potassium, magnesium, aluminum, zinc, silver, sodium, titanium, each 0.01 μ g/ml.
Embodiment 1
Use plate ice machine that deionized water is prepared into ice.
In the reaction chamber, sample cell is placed with 150cm3Ice, sample room liquid nitrogen refrigerating, maintain the temperature at less than-75 DEG C.Receiving chamber is put into 100mL not aqueous cosmetics emulsion, utilizes mechanical pump and molecular pump evacuation, make vacuum in reative cell reach 2 × 10-2Pa.Opening laser instrument, carry out laser splash and produce small water molecule cluster, the produced optical maser wavelength of laser instrument is 1064nm, and laser energy is 20mJ；Open the valve of pipeline between gas bomb and reative cell, in reative cell, noble gas is passed into by stainless steel pipes, open the agitator in magnetic field generator and receiving chamber, the magnetic induction 0.05T in magnetic field is set, frequency is 20kHz, agitator speed is 50rpm, and whole flow process continues 1 hour, regulates laser position once every 10 minutes.
Finally give the emulsion of following formula, with parts by weight: microcrystalline wax 1, Cera Flava 2, lanoline 2, liquid paraffin 20, isotriacontane 10, Span-83 4, polyoxyethylene (20) sorbitan monooleate 1, propylene glycol 7, small water molecule cluster (TMW) 53.
Embodiment 2
Use plate ice machine that deionized water is prepared into ice.In the reaction chamber, sample cell is placed with 150cm3Ice, sample room liquid nitrogen refrigerating, maintain the temperature at less than-75 DEG C.Receiving chamber is put into 100mL not aqueous cosmetics emulsion, utilizes mechanical pump and molecular pump evacuation, make vacuum in reative cell reach 2 × 10-1Pa.Opening laser instrument, carry out laser splash and produce small water molecule cluster, the produced optical maser wavelength of laser instrument is 1064nm, and laser energy is 20mJ；Open the valve of pipeline between gas bomb and reative cell, in reative cell, noble gas is passed into by stainless steel pipes, open the agitator in magnetic field generator and receiving chamber, the magnetic induction 0.05T in magnetic field is set, frequency is 20kHz, agitator speed is 50rpm, and whole flow process continues 1 hour, regulates laser position once every 10 minutes.
Finally give the emulsion of following formula, with parts by weight: microcrystalline wax 1, Cera Flava 2, lanoline 2, liquid paraffin 20, isotriacontane 10, Span-83 4, polyoxyethylene (20) sorbitan monooleate 1, propylene glycol 7, small water molecule cluster (TMW) 53.
Embodiment 3
Use plate ice machine that deionized water is prepared into ice.In the reaction chamber, sample cell is placed with 150cm3Ice, sample room liquid nitrogen refrigerating, maintain the temperature at less than-75 DEG C.Receiving chamber is put into 100mL not aqueous cosmetics emulsion, utilizes mechanical pump and molecular pump evacuation, make vacuum in reative cell reach 8 × 10-3Pa.Opening laser instrument, carry out laser splash and produce small water molecule cluster, the produced optical maser wavelength of laser instrument is 1064nm, and laser energy is 20mJ；Open the valve of pipeline between gas bomb and reative cell, in reative cell, noble gas is passed into by stainless steel pipes, open the agitator in magnetic field generator and receiving chamber, the magnetic induction 0.05T in magnetic field is set, frequency is 20kHz, agitator speed is 50rpm, and whole flow process continues 1 hour, regulates laser position once every 10 minutes.
Finally give the emulsion of following formula, with parts by weight: microcrystalline wax 1, Cera Flava 2, lanoline 2, liquid paraffin 20, isotriacontane 10, Span-83 4, polyoxyethylene (20) sorbitan monooleate 1, propylene glycol 7, small water molecule cluster (TMW) 53.
Embodiment 4
Use plate ice machine that deionized water is prepared into ice；In the reaction chamber, sample cell is placed with 150cm3Ice, sample room liquid nitrogen refrigerating, maintain the temperature at less than-75 DEG C.Receiving chamber is put into 100mL not aqueous cosmetics emulsion, utilizes mechanical pump and molecular pump evacuation, make vacuum in reative cell reach 2 × 10-2Pa.Opening laser instrument, carry out laser splash and produce small water molecule cluster, the produced optical maser wavelength of laser instrument is 1064nm, and laser energy is 50mJ；Open the valve of pipeline between gas bomb and reative cell, in reative cell, noble gas is passed into by stainless steel pipes, open the agitator in magnetic field generator and receiving chamber, the magnetic induction 0.05T in magnetic field is set, frequency is 20kHz, agitator speed is 50rpm, and whole flow process continues 0.6 hour, regulates laser position once every 8 minutes.
Finally give the emulsion of following formula, with parts by weight: microcrystalline wax 1, Cera Flava 2, lanoline 2, liquid paraffin 20, isotriacontane 10, Span-83 4, polyoxyethylene (20) sorbitan monooleate 1, propylene glycol 7, small water molecule cluster (TMW) 53.
Embodiment 5
Use plate ice machine that deionized water is prepared into ice；In the reaction chamber, sample cell is placed with 150cm3Ice, sample room liquid nitrogen refrigerating, maintain the temperature at less than-75 DEG C.Receiving chamber is put into 100mL not aqueous cosmetics emulsion, utilizes mechanical pump and molecular pump evacuation, make vacuum in reative cell reach 2 × 10-2Pa.Opening laser instrument, carry out laser splash and produce small water molecule cluster, the produced optical maser wavelength of laser instrument is 1064nm, and laser energy is 10mJ；Open the valve of pipeline between gas bomb and reative cell, in reative cell, noble gas is passed into by stainless steel pipes, open the agitator in magnetic field generator and receiving chamber, the magnetic induction 0.05T in magnetic field is set, frequency is 20kHz, agitator speed is 50rpm, and whole flow process continues 1 hour, regulates laser position once every 10 minutes.
Finally give the emulsion of following formula, with parts by weight: microcrystalline wax 1, Cera Flava 2, lanoline 2, liquid paraffin 20, isotriacontane 10, Span-83 4, polyoxyethylene (20) sorbitan monooleate 1, propylene glycol 7, small water molecule cluster (TMW) 53.
Embodiment 6
Use plate ice machine that deionized water is prepared into ice；In the reaction chamber, sample cell is placed with 150cm3Ice, sample room liquid nitrogen refrigerating, maintain the temperature at less than-75 DEG C.Receiving chamber is put into 100mL not aqueous cosmetics emulsion, utilizes mechanical pump and molecular pump evacuation, make vacuum in reative cell reach 2 × 10-2Pa.Opening laser instrument, carry out laser splash and produce small water molecule cluster, the produced optical maser wavelength of laser instrument is 355nm, and laser energy is 20mJ；Open the valve of pipeline between gas bomb and reative cell, in reative cell, noble gas is passed into by stainless steel pipes, open the agitator in magnetic field generator and receiving chamber, the magnetic induction 0.05T in magnetic field is set, frequency is 20kHz, agitator speed is 50rpm, and whole flow process continues 1 hour, regulates laser position once every 10 minutes.
Finally give the emulsion of following formula, with parts by weight: microcrystalline wax 1, Cera Flava 2, lanoline 2, liquid paraffin 20, isotriacontane 10, Span-83 4, polyoxyethylene (20) sorbitan monooleate 1, propylene glycol 7, small water molecule cluster (TMW) 53.
Embodiment 7
Use plate ice machine that deionized water is prepared into ice；In the reaction chamber, sample cell is placed with 150cm3Ice, sample room liquid nitrogen refrigerating, maintain the temperature at less than-75 DEG C.Receiving chamber is put into 100mL not aqueous cosmetics emulsion, utilizes mechanical pump and molecular pump evacuation, make vacuum in reative cell reach 2 × 10-2Pa.Opening laser instrument, carry out laser splash and produce small water molecule cluster, the produced optical maser wavelength of laser instrument is 532nm, and laser energy is 20mJ；Open the valve of pipeline between gas bomb and reative cell, in reative cell, noble gas is passed into by stainless steel pipes, open the agitator in magnetic field generator and receiving chamber, the magnetic induction 0.05T in magnetic field is set, frequency is 20kHz, agitator speed is 50rpm, and whole flow process continues 1 hour, regulates laser position once every 10 minutes.
Finally give the emulsion of following formula, with parts by weight: microcrystalline wax 1, Cera Flava 2, lanoline 2, liquid paraffin 20, isotriacontane 10, Span-83 4, polyoxyethylene (20) sorbitan monooleate 1, propylene glycol 7, small water molecule cluster (TMW) 53.
Embodiment 8
Use plate ice machine that deionized water is prepared into ice；In the reaction chamber, sample cell is placed with 150cm3Ice, sample room liquid nitrogen refrigerating, maintain the temperature at less than-75 DEG C.Receiving chamber is put into 100mL not aqueous cosmetics emulsion, utilizes mechanical pump and molecular pump evacuation, make vacuum in reative cell reach 2 × 10-2Pa.Opening laser instrument, carry out laser splash and produce small water molecule cluster, the produced optical maser wavelength of laser instrument is 1064nm, and laser energy is 20mJ；Open the valve of pipeline between gas bomb and reative cell, in reative cell, noble gas is passed into by stainless steel pipes, open the agitator in magnetic field generator and receiving chamber, the magnetic induction 0.8T in magnetic field is set, frequency is 20kHz, agitator speed is 50rpm, and whole flow process continues 1 hour, regulates laser position once every 10 minutes.
Finally give the emulsion of following formula, with parts by weight: microcrystalline wax 1, Cera Flava 2, lanoline 2, liquid paraffin 20, isotriacontane 10, Span-83 4, polyoxyethylene (20) sorbitan monooleate 1, propylene glycol 7, small water molecule cluster (TMW) 53.
Embodiment 9
Use plate ice machine that deionized water is prepared into ice；In the reaction chamber, sample cell is placed with 150cm3Ice, sample room liquid nitrogen refrigerating, maintain the temperature at less than-75 DEG C.Receiving chamber is put into 100mL not aqueous cosmetics emulsion, utilizes mechanical pump and molecular pump evacuation, make vacuum in reative cell reach 2 × 10-2Pa.Opening laser instrument, carry out laser splash and produce small water molecule cluster, the produced optical maser wavelength of laser instrument is 1064nm, and laser energy is 20mJ；Open the valve of pipeline between gas bomb and reative cell, in reative cell, noble gas is passed into by stainless steel pipes, open the agitator in magnetic field generator and receiving chamber, the magnetic induction 0.003T in magnetic field is set, frequency is 20kHz, agitator speed is 50rpm, and whole flow process continues 1 hour, regulates laser position once every 10 minutes.
Finally give the emulsion of following formula, with parts by weight: microcrystalline wax 1, Cera Flava 2, lanoline 2, liquid paraffin 20, isotriacontane 10, Span-83 4, polyoxyethylene (20) sorbitan monooleate 1, propylene glycol 7, small water molecule cluster (TMW) 53.
Embodiment 10
Use plate ice machine that deionized water is prepared into ice；In the reaction chamber, sample cell is placed with 150cm3Ice, sample room liquid nitrogen refrigerating, maintain the temperature at less than-75 DEG C.Receiving chamber is put into 100mL not aqueous cosmetics emulsion, utilizes mechanical pump and molecular pump evacuation, make vacuum in reative cell reach 2 × 10-2Pa.Opening laser instrument, carry out laser splash and produce small water molecule cluster, the produced optical maser wavelength of laser instrument is 1064nm, and laser energy is 20mJ；Open the valve of pipeline between gas bomb and reative cell, in reative cell, noble gas is passed into by stainless steel pipes, open the agitator in magnetic field generator and receiving chamber, the magnetic induction 0.05T in magnetic field is set, frequency is 50kHz, agitator speed is 50rpm, and whole flow process continues 1 hour, regulates laser position once every 10 minutes.
Finally give the emulsion of following formula, with parts by weight: microcrystalline wax 1, Cera Flava 2, lanoline 2, liquid paraffin 20, isotriacontane 10, Span-83 4, polyoxyethylene (20) sorbitan monooleate 1, propylene glycol 7, small water molecule cluster (TMW) 53.
Embodiment 11
Use plate ice machine that deionized water is prepared into ice；In the reaction chamber, sample cell is placed with 150cm3Ice, sample room liquid nitrogen refrigerating, maintain the temperature at less than-75 DEG C.Receiving chamber is put into 100mL not aqueous cosmetics emulsion, utilizes mechanical pump and molecular pump evacuation, make vacuum in reative cell reach 2 × 10-2Pa.Opening laser instrument, carry out laser splash and produce small water molecule cluster, the produced optical maser wavelength of laser instrument is 1064nm, and laser energy is 20mJ；Open the valve of pipeline between gas bomb and reative cell, in reative cell, noble gas is passed into by stainless steel pipes, open the agitator in magnetic field generator and receiving chamber, the magnetic induction 0.05T in magnetic field is set, frequency is 5kHz, agitator speed is 50rpm, and whole flow process continues 1 hour, regulates laser position once every 10 minutes.
Finally give the emulsion of following formula, with parts by weight: microcrystalline wax 1, Cera Flava 2, lanoline 2, liquid paraffin 20, isotriacontane 10, Span-83 4, polyoxyethylene (20) sorbitan monooleate 1, propylene glycol 7, small water molecule cluster (TMW) 53.
Embodiment 12
Take the mineral water containing, for example lower metallic element: each 0.01 μ g/ml of ferrum, potassium, magnesium, aluminum, zinc, silver, sodium, titanium；Use plate ice machine that described mineral water is prepared into ice.Prepare small water molecule cluster by method described in embodiment 1, and mix with not aqueous cosmetics emulsion.Finally give the emulsion of following formula, with parts by weight: microcrystalline wax 1, Cera Flava 2, lanoline 2, liquid paraffin 20, isotriacontane 10, Span-83 4, polyoxyethylene (20) sorbitan monooleate 1, propylene glycol 7, small water molecule cluster (TMW) 53.
Embodiment 13
Take from water, use plate ice machine to prepare into ice, adopt method described in embodiment 1 to prepare small water molecule cluster, and mix with not aqueous cosmetics emulsion.Finally give the emulsion of following formula, with parts by weight: microcrystalline wax 1, Cera Flava 2, lanoline 2, liquid paraffin 20, isotriacontane 10, Span-83 4, polyoxyethylene (20) sorbitan monooleate 1, propylene glycol 7, small water molecule cluster (TMW) 53.
Comparative example 1
Choose the usual ingredients being made by cosmetic emulsion, with parts by weight: microcrystalline wax 1, Cera Flava 2, lanoline 2, liquid paraffin 20, isotriacontane 10, Span-83 4, polyoxyethylene (20) sorbitan monooleate 1, propylene glycol 7, light water 53.The technology adopting conventional homogenizer prepares into common cosmetic emulsion.
Comparative example 2
Use plate ice machine that deionized water is prepared into ice.
In the reaction chamber, sample cell is placed with 150cm3Ice, sample room liquid nitrogen refrigerating, maintain the temperature at less than-75 DEG C.Putting into 100mL not aqueous cosmetics emulsion in receiving chamber, reative cell is under normal pressure.Opening laser instrument, carry out laser splash and produce small water molecule cluster, the produced optical maser wavelength of laser instrument is 1064nm, and laser energy is 20mJ；Open the valve of pipeline between gas bomb and reative cell, in reative cell, noble gas is passed into by stainless steel pipes, open the agitator in magnetic field generator and receiving chamber, the magnetic induction 0.05T in magnetic field is set, frequency is 20kHz, agitator speed is 50rpm, and whole flow process continues 1 hour, regulates laser position once every 10 minutes.
Finally give the emulsion of following formula, with parts by weight: microcrystalline wax 1, Cera Flava 2, lanoline 2, liquid paraffin 20, isotriacontane 10, Span-83 4, polyoxyethylene (20) sorbitan monooleate 1, propylene glycol 7, small water molecule cluster (TMW) 53.
Method of testing
(1) adopt and test small water molecule cluster with the following method to the anti-reflection coefficient of active component in cosmetics, measurement adds the efficiency that the cosmetics of small water molecule cluster (TMW) are absorbed by the skin, and characterizes the small water molecule cluster (TMW) the short effect to cosmetics effective active composition.
Short saturating material: small water molecule cluster (TMW)
Model composition in cosmetics: isotriacontane
Use the Transdermal absorption instrument that Tianjin silicon new science and technology company limited produces and the Agilent1100 high performance liquid chromatograph that Aglient company produces, nude mice animal skin is tested.
Take the nude mice of 10 week old, body weight 20 ± 9g, male, 9, disconnected neck is put to death, isolate xiphoid-process hypogastric region skin, carefully reject subcutaneous tissue and fat, be sandwiched in microscope slide after cleaning with physiological saline solution, it is stored in-20 DEG C--in the cryogenic refrigerator of 30 DEG C, standby, because every piece of skin is variant, therefore as far as possible with the skin of abdomen of a nude mice.
Experiment packet: matched group 1 group, short saturating substance migration light water, sample sets 1 group, small water molecule cluster (TMW) prepared by short saturating substance migration the method for the invention.
Experimental technique: take isolated skin and be fixed in the middle of diffusion cell, area 0.825cm2Make stratum corneum side to supply pool, supply pool adds a certain amount of supply solution (filtering with 0.45um microporous filter membrane), acceptance pool adds 5ml acceptable solution, diffusion cell water bath with thermostatic control water temperature is 36 ± 0.5 DEG C (cell rotating speed: 500r/min), stirrer adds in diffusion cell, weighing apparatus speed stirring.
Start timing after application of sample 15min, sample 1ml respectively at 0h, 1h, 2h, 4h, 6h, 8h, 12h, 24h, and supplement equivalent acceptable solution immediately, make acceptable solution remain at 5ml capacity, after sample filters with microporous filter membrane, with the content of HPLC testing index composition.And it is calculated as follows correction drug level CnSchool, unit are accumulation infiltration capacity Q, stable state transmission rates Js, infiltration coefficient P.
CN school=CN surveys+0.2/5∑Cp
Wherein CN school: calibration model constituent concentration；Cn: actually measured model constituent concentration；
∑ Cp: the mensuration concentration sum of each point before each sampling；
Q=CN school×V/A
With the Q of different time, time t being mapped, the straight line portion slope of this figure is stable state transmission rates Js.
P=Js/C0
Wherein P: infiltration coefficient；A: diffusion cell cross-sectional area；V: acceptable solution volume in acceptance pool；C0: for die trial type constituent concentration in supply pool.
Anti-reflection coefficient=P sample sets/P matched group
Assay chromatographic condition:
Chromatographic column: with octadecylsilane chemically bonded silica for filler, HYPERSILC18Post (4.6 × 300mm, 5 μ)；Mobile phase: for methanol-water (85: 15)；Flow velocity: 1ml min-1；Detection wavelength: 270nm；Sample size: 10 μ l.
Test result
Under this experiment condition, the addition of small water molecule cluster (TMW) can promote the skin absorption of cosmetic actives.Compared with matched group, sample sets can increase infiltration rate and the Percutaneous permeability of this composition.
(2) moistening effect
Choose healthy volunteer 100, men and women half and half, 20～60 years old age, disease without serious systemic, without immunodeficiency or autoimmune disease, without activeness anaphylactic disease, to skin-care cosmetics without severe allergy history, do not use hormone medicine or immunosuppressant in nearly one month, do not participated in other clinical trials, and do not smeared the external preparation such as any cosmetics, experimentation keeps original rule of life.
Test all experimenters, moisture after skin uses emulsion 6 hours and water loss amount, average.
Use moisture of skin measuring instrument CorneometerCM825 to test skin beauty water and state, test the water loss amount of skin through skin moisture loss measuring instrument TewameterTM300.
(3) whitening effect
Choose healthy volunteer 100, men and women half and half, 20～60 years old age, disease without serious systemic, without immunodeficiency or autoimmune disease, without activeness anaphylactic disease, to skin-care cosmetics without severe allergy history, do not use hormone medicine or immunosuppressant in nearly one month, do not participated in other clinical trials, and do not smeared the external preparation such as any cosmetics, experimentation keeps original rule of life.Test subjects skin uses the change of emulsion skin complexion L-value after 2 months and the change of melanin value H to carry out whitening effect assessment.
Skin complexion measures: use the skin color tester ColorimeterCL400 that German Courage+Khazaka (CK) company produces to measure the mensuration of target site skin complexion L-value, uses the change of front and back skin L-value to assess the impact on the bright degree of skin of this product by measuring product.△ L-value is more big, and whitening effect is more good.
The mensuration of dermal melanin: use the dermal melanin of Courage+Khazaka (CK) company of Germany production and haemachrome measuring instrument MX18 to measure melanin value H in skin, target site dermal melanin is measured 5 times, take its meansigma methods, use by measuring product the change of front and back dermal melanin numerical value to assess the skin whitening efficacy of this product.△ H-number is more little, and whitening effect is more good.
Test result is in Table 1
Table 1
As can be seen from the above data, method of the present invention is adopted to prepare small water molecule cluster (TMW), cosmetic active can be significantly improved, effective ingredient in cosmetics is had significantly short saturating performance by small water molecule cluster (TMW), and compared with the cosmetics without small water molecule cluster (TMW), all it is obviously improved containing the moisturizing of cosmetics of small water molecule cluster (TMW), moisturizing and whitening effect.
Above-described embodiment is merely illustrative, for explaining feature and the application mode of the method for the invention, can not be used for limiting the present invention, appended claim is intended to the scope wide as far as possible that requirement it is contemplated that, variant such as the term " comprising " used in the claims and its meaning of one's words in theory also includes different expression waies, for instance but it is not limited to " it consists of ".Embodiment as herein described is only the embodiment that part is possible.Therefore, the claim appended by the present invention is not by described example limitation.Some numerical rangies used in the claims also include subrange within, and the change in these scopes also should be construed to be covered by appended claim in the conceived case.
Claims (10)
1. the preparation method of the small water molecule cluster TMW promoting cosmetic active, it is characterised in that comprise the steps of
(1) ice is prepared in aqueous water freezing；
(2) under vacuum, utilizing laser splash ice, produce small water molecule cluster TMW, described small water molecule cluster TMW is plasma state.
2. the preparation method of a kind of small water molecule cluster TMW promoting cosmetic active according to claim 1, it is characterized in that, one or more in following material of aqueous water in described step (1): distilled water, deionized water, mineral water, tap water.
3. the preparation method of a kind of small water molecule cluster TMW promoting cosmetic active according to claim 2, it is characterised in that described mineral water comprises one or more in following metallic element: ferrum, potassium, magnesium, aluminum, zinc, silver, sodium, titanium.
4. the preparation method of a kind of small water molecule cluster TMW promoting cosmetic active according to claim 1, it is characterised in that in described step (2), the vacuum of vacuum condition is 2 × 10-1Pa～8 × 10-3Pa。
5. the preparation method of a kind of small water molecule cluster TMW promoting cosmetic active according to claim 1, it is characterised in that in described step (2), the optical maser wavelength for sputtering is the one in 266nm, 355nm, 532nm, 1064nm.
6. the preparation method of a kind of small water molecule cluster TMW promoting cosmetic active according to claim 5, it is characterised in that the described optical maser wavelength for sputtering is 1064nm.
7. the preparation method of a kind of small water molecule cluster TMW promoting cosmetic active according to claim 6, it is characterised in that the described laser energy for sputtering is 10～50mJ.
8. cosmetics, it is characterised in that comprise small water molecule cluster TMW prepared by the method described in any one of claim 1～7.
9. the preparation method of cosmetics, it is characterised in that comprise the steps of and be placed in magnetic field by cosmetics, under being stirred continuously, deposits to small water molecule cluster TMW prepared by the method described in any one of claim 1～7 in cosmetics.
10. the preparation method of a kind of cosmetics according to claim 9, it is characterised in that the magnetic induction in described magnetic field is 0.003～0.8T, frequency is 5～50kHz.
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