CN109303726A - A kind of preparation method and application of ceramide promotor - Google Patents
A kind of preparation method and application of ceramide promotor Download PDFInfo
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- CN109303726A CN109303726A CN201811360496.8A CN201811360496A CN109303726A CN 109303726 A CN109303726 A CN 109303726A CN 201811360496 A CN201811360496 A CN 201811360496A CN 109303726 A CN109303726 A CN 109303726A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/4906—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with one nitrogen as the only hetero atom
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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- 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
- A61Q19/08—Anti-ageing preparations
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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
- A61K2800/84—Products or compounds obtained by lyophilisation, freeze-drying
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Abstract
The invention discloses a kind of preparation method and applications of ceramide promotor, are related to bioactive substance preparation and application technical field.The ceramide promotor screens pineapple leaves, Radix Paeoniae Alba, motherwort, oolong tea is as raw material, azone, menthol, cubeb oil is as auxiliary material, raw material is scientifically and rationally designed to choose and pre-process, it is heat-treated in short-term, freeze-drying, it crushes, extract concentration, filter residue extracts again, the process route of auxiliary material addition, the percutaneous absorbability of the ceramide promotor is good, effective component extraction rate is high in raw material, reduce cost of material, the experiment proved that having effects that good promotion ceramide generates, and it can significantly improve face wrinkles, enhance moisturizing moisturizing and the barrier function of face.
Description
Technical field
The present invention relates to bioactive substance preparation and application technical fields, and in particular to a kind of ceramide promotor
Preparation method and application.
Background technique
Ceramide is micro existing lipid in organism entirety, but accounts for rouge in the outermost layer cuticula of skin
More than half of matter plays an important role in the moisturizing mechanism of skin, barrier mechanism.In addition, in recent years by promoting mind
Through amide generate and induce cell apoptosis, induction, Proliferation Ability phenomenon also have been reported that, to diseases associated with inflammation, malignant tumour
Etc. the therapeutic effect of cell proliferation and differentiation disease caused by reasons need further to study.Also studies have reported that ceramide
Inhibiting effect is reduced with bone resorption inhibiting effect, bone invigoration effect, alveolus, to osteoporosis, fracture, pain in the loins, rheumatism etc.
Bone and joint diseases have prevention and improvement result.
Although skin has the ability for generating ceramide, production capacity is limited, it is desirable to reach good skin moisture-keeping screen
Hinder effect, it is also necessary to introduce ceramide-analogous or ceramide promotor.It is known that glucose ceramide, gala
The sphingolipids constituents such as glycosyl ceramide have the ability for promoting cuticula to keep moisture, improve skin roughness.Application number
200780040739.3 patent discloses grape sap as effective component and synthesizes ceramide promotor and by the promotor
It is applied to cosmetics and skin preparations for extenal use.The patent of application number 200910118747.6 is provided with the plant of motherwort, Chinese yam
Or ceramide production accelerant of the extract as effective component, moisturizer.The patent of application number 200910118746.1 is public
Having opened plant or its extract selected from the root of Dahurain angelica, glutinous rehmannia, Rhizoma Atractylodis Macrocephalae, Radix Glycyrrhizae, rheum officinale, bletilla, the fleece-flower root and campanulaceae is effective component
Ceramide production accelerant.
Ceramide promotor disclosed above or preparation method have the following problems: 1, ceramide substance is most
For water-insoluble materials, and the prior art selects Chinese medicine water extracting component or petroleum ether extract component, polarity excessive or too small, no
It is easy Transdermal absorption and generates facilitation；2, preparation process be all made of simple low temperature extract, filtering, concentration, do not disclose
The pre-treatment of herbal medicine, drying, crushing process, although technique is simple, effective component extraction efficiency is low, increase raw material at
This.
Summary of the invention
In order to overcome above-mentioned technical problem, the purpose of the present invention is to provide a kind of preparation sides of ceramide promotor
Method and application, screening pineapple leaves, Radix Paeoniae Alba, motherwort, oolong tea are as raw material, and azone, menthol, cubeb oil are as auxiliary
Material scientifically and rationally designs raw material and chooses with pretreatment, heat treatment in short-term, be freeze-dried, crush, extracting concentration, filter residue again
It extracts, the process route of auxiliary material addition, the percutaneous absorbability of the ceramide promotor is good, effective component extraction rate in raw material
Height reduces cost of material, the experiment proved that having effects that good promotion ceramide generates, and can significantly improve
Face wrinkles enhance moisturizing moisturizing and the barrier function of face.
The purpose of the present invention can be achieved through the following technical solutions:
The present invention provides a kind of preparation methods of ceramide promotor, comprising the following steps:
1) raw material is chosen and is pre-processed: in parts by weight, weighing 80-120 parts of pineapple leaves, 12-18 parts of Radix Paeoniae Alba, motherwort
20-28 parts, 5-11 parts of oolong tea；Wherein, pineapple leaves are selected from growth two months or more 1 year, immature pineapple, after pretreatment
Standing drains away the water；Radix Paeoniae Alba, motherwort, oolong tea are robbed water and are cleaned, and are dried for standby；
The present invention is when choosing the raw material of ceramide promotor, " CHINA JOURNAL OF CHINESE MATERIA MEDICA " phase entitled " spinach of volume 32 the 5th
The article of new amide constituents in trailing plants leaf " discloses a kind of method for studying chemical component in pineapple leaves, determines that structure is 1-
Positive 16 carbon -4,10 (E, E) of positive 22 carbonic acyl radical-of O- β-D-Glucose-N--diene sphingol glycosides, illustrates to contain in pineapple leaves
There is ceramide-analogous, there may be facilitation to the generation of ceramide.It helps digestion modern research shows that pineapple leaves have
Stomach function regulating, antidiarrheal and other effects can be used for indigestion, epigastric distending pain, summer heat and rushes down, and also have Adjust-blood lipid, hypoglycemic, the protection heart
The multiple pharmacological effects such as dirty, antitumor, antibacterial, anti-oxidant.
Radix Paeoniae Alba is the dry root of ranunculaceae plant Chinese herbaceous peony, summer, the excavation of two season of autumn, is cleaned, and removes end to end and radicula, sets boiling
It boils, dries again after removing crust or peeling after boiling in water.[nature and flavor] are bitter, acid, slightly cold.[channel tropism] liver, the spleen channel.[function master
Control] blood-nourishing and battalion；Relieving spasm to stop pain；Hold back high and level tone liver.Main irregular menstruation；Dysmenorrhea；Metrorrhagia and metrostaxis；Spontaneous perspiration；Night sweat；Side of body rib stomach duct and abdomen pain
Bitterly；Four limbs contraction pain；Headache；Dizziness.Clinic it has been confirmed that pharmacological action have central inhibitory action, spasmolysis, anti-inflammatory anti-burst
Ulcer acts on, to booster action, antibacterial action, protecting liver and detoxication effect of cardiovascular system etc..
Motherwort is the herb of Lamiaceae plant motherwort.Summer riotous growth and flower non-standard-sized sheet when, extract aerial part,
It dries.[nature and flavor] are bitter, pungent, slightly cold.[channel tropism] liver, pericardium channel.[major function] promoting blood circulation for regulating menstruation, inducing diuresis to remove edema.Not for menstruation
It adjusts, dysmenorrhea, menostasis, lochiorrhagia, edema and little urine；Acute nephritis edema.It is female containing leonurine, stachydrine, benefit in motherwort
A variety of alkaloids such as the fixed, leonurinine of grass, benzoic acid, volume potassium chloride, lauric acid, linolenic acid, oleic acid, sterol, vitamin A,
The flavonoids such as rutin, and contain arginine, 4- guanidine radicals-n-butyl alcohol, 4- guanidine radicals-butyric acid, stachyose.Motherwort water soluble ingredient without
All there is excitation by the uterus in vitro, in place and whole not anesthetized animal, but its real effectively alkaloid waits to determine.
Oolong tea is also known as green tea, semi-fermented tea and full fermentation tea, and kind is more, is unique distinctness in several big teas of China
The tealeaves category of distinct Chinese characteristics.Oolong tea is the product produced after the processes such as pick, wither, leaf rotation, fried green, rub, bake
Different teas of fine quality.Containing organic chemical composition up to more than 450 kinds in oolong tea, inorganic mineral element is up to more than 40 kinds.It is organic
Chemical component mainly has: tea polyphenols, vegetable soda, protein, amino acid, vitamin, pectin element, organic acid, lipopolysaccharides, sugar
Class, enzyme, pigment etc..In addition to general tealeaves there is benefit of refreshing oneself to think, elimination fatigue, diuresis of promoting the production of body fluid, antipyretic sunstroke prevention, sterilization disappear
Outside the healthcare functions such as scorching, dispelling cold relieves the effect of alcohol, diseases prevention of detoxify, promoting digestion greasy, defatting beauty, and also outstanding behaviours anti-cancer, reducing blood lipid,
The special efficacies such as anti-aging.
2) it is heat-treated in short-term: pretreated pineapple leaves, Radix Paeoniae Alba, motherwort, oolong tea is sent into steam rotary dryer
In, it is passed through 60 ± 5 DEG C of hot steam processing 3-5min, cooled to room temperature；
In short-term in heat treatment process, 60 ± 5 DEG C of hot steam processing will not make the excessive thermal expansion pore of raw material, thermal sensitivity object
Matter, protein, vitamin are also unlikely to heated denaturalization, reduce remaining water content, and being cooled to room temperature rear active constituent will not
Inactivation.
3) be freeze-dried, crush: pineapple leaves, Radix Paeoniae Alba, motherwort, oolong tea are sent into vacuum freeze drier, at -10 DEG C
~-5 DEG C of freeze-drying 1-2h；Pulverizer precomminution is put into graininess, 20-40 mesh is crossed, removes fine powder, pulverize
Obtain 8-12 μm of partial size of mixing fine powders；
In freezing dry process, raw material can be frozen into solid, then come out steam sublimation under vacuum conditions,
Heat-sensitive substance, protein, vitamin isoreactivity substance can be left in the ice shelf freezed, it is dry after volume difference it is small, be in
Existing loose porous structure, and oxygen is few under low temperature, is easy the phenolic substances being oxidized by oxygen, N- ester acyl sphingosine class
Substance will not be oxidized inactivation, remain active material to the maximum extent.In crushing process, the flavones of non-refractory can be retained
The bioactive ingredients such as class, glycoside, carbohydrate, volatile oil sufficiently crush broken wall to the cell of Chinese medicine, promote releasing for active constituent
It puts and dissolves out, increase specific surface area, improve bioavilability.
4) extract concentration: mixing fine powders are added in multi-function extractor, and 8 times of 75% ethyl alcohol of amount, refluxing extraction 1- is added
2h adds 4 times of 85% ethyl alcohol of amount, refluxing extraction 40-60min, combined extract；Extracting solution vacuum suck single-effect external circulation is dense
In contracting tank, it is concentrated under reduced pressure and removes 3/4 ethyl alcohol, filtrate and filter residue is obtained by filtration；
It extracts in concentration process, is first extracted using the ethyl alcohol of large dosage of low concentration, reuse low dose of high concentration
Ethyl alcohol extracts.On the one hand, the leaf skin mixing fine powders of small particle are pulverizing the abundant broken wall of process, and effective component is
Substantially it is discharged, carries out alcohol extracting without a large amount of high concentration ethanol；On the other hand, the contact area of low-concentration ethanol and fine powder
Greatly, Alcohol soluble composition recovery rate is high, reuses high concentration ethanol, supplements the ethyl alcohol evaporated, increases concentration of alcohol, extracts
The poor active material of alcohol-soluble, after the concentration of two step extracting solutions, the high blending constituent of available activity substance content.It depressurizes dense
After contracting removes 3/4 ethyl alcohol, filtering, so that remaining ethyl alcohol has dissolved most of alcohol-soluble effective component.
5) filter residue extracts again: the filter residue of step 4) being added to the water of 10 times of amounts, is stirred evenly, 6 times of amount petroleum are successively used
Ether carries out single extraction, and 4 times of amount ethyl acetate carry out reextraction, and 4 times of amount ethyl alcohol are extracted three times；Collect reextraction and
The oily phase extracted three times, is concentrated under reduced pressure, and 0.5 μm of nanofiltration membrane obtains pale tan oil；
For filter residue again in extraction process, single extraction uses small polarity petroleum ether, can remove the small polar impurity in filter residue,
Ethyl acetate is close with ethyl alcohol polarity and dissolubility is good, can extract remaining alcohol-soluble effective component in filter residue, further
Increase the utilization rate of extraction efficiency and raw material.
6) auxiliary material adds: the pale tan oil of the filtrate of step 4), step 5) being mixed, concentration removes ethyl alcohol and mixed
Object A is closed, mixture A is uniformly mixed with suitable azone, menthol, cubeb oil.
For the present invention in auxiliary material addition step, azone can change skin chromaticness layer lipid and protein structure, promote
The Transdermal absorption of drug can enhance transdermal effect to hydrophily and hydrophobic compound；Menthol is also known as menthol, belongs to
In hexamethylene monoterpene derivative, research finds that containing menthol compound penetration enhancer is remarkably improved transdermal enhancing effect；Piper cubeba system
The dry mature fruit of Lauraceae Litsea plant cubeb litsen tree also known as the fruit of a cubeb litsea tree, volatile oil content are high, can be with azone
Play collaboration transdermal enhancing effect.The present invention has carried out a large amount of screening and experiment to the type and dosage of transdermal enhancer, and laurel is worked as in discovery
Azone, menthol, cubeb oil dosage when being respectively 3-5%, 4-6%, 6-8% of mixture A mass, can play good
Mixing promote saturating effect.
As a further solution of the present invention, step 1) the pineapple leaves pretreatment specifically: cut into 1-3cm strip
Shape infiltrates 20-30min using the sodium carbonate liquor of 6-8wt%, is put into the ultrasonic cleaner for being loaded with purified water after taking-up
It is ultrasonically treated 5-8min.
In pineapple leaves preprocessing process, the specific surface area that strip increases pineapple leaves is cut into, in sodium carbonate liquor
In impregnation process, the contact area with solution is increased, while being conducive to the dust and pesticide on removal surface, makes adherency in pineapple leaves
Colloid substance pineapple proteinase hydrolyze under alkaline condition, conducive to the release of active material in subsequent handling.Ultrasonic cleaning can
To make pineapple leaves sodium carbonate liquor diffusion dissolution remained on surface in water by ultrasonic cavitation effect phenomenon, make mutability object
Matter pineapple organic acid is dissolved in the water, conducive to the extraction separation of active material in subsequent handling.
As a further solution of the present invention, the step 3), which pulverizes, uses airslide disintegrating mill, and grinding tolerance is 6-
10m3/ min, air pressure 0.7-1.0MPa, tappered rating 5.5kW.
As a further solution of the present invention, vacuum degree is -0.08~-0.05MPa, temperature when the step 4) is concentrated under reduced pressure
Degree is 45-52 DEG C, steam pressure 0.08-0.12MPa.
As a further solution of the present invention, the centrifuge separation of 1-2min is carried out when the step 5) single extraction, it is secondary
The centrifuge separation that 40-60s is carried out when extraction, carries out the centrifuge separation of 20-30s when extracting three times.
As a further solution of the present invention, the step 6) azone, menthol, cubeb oil dosage be respectively
3-5%, 4-6%, 6-8% of mixture A mass.
The present invention also provides above-mentioned ceramide promotors to improve the application on face wrinkles.
Beneficial effects of the present invention:
1, the preparation method of ceramide promotor of the invention, select pineapple leaves, Radix Paeoniae Alba, motherwort, oolong tea as
Raw material, azone, menthol, cubeb oil scientifically and rationally design raw material and choose and pre-process, is hot in short-term as auxiliary material
Processing, freeze-drying, crushing, extraction is concentrated, filter residue extracts again, the process route of auxiliary material addition, the ceramide promotor
Percutaneous absorbability is good, and effective component extraction rate is high in raw material, reduces cost of material, the experiment proved that having good promotion mind
The effect of being generated through amide, and just can significantly improve face wrinkles after mixing with skin care item, cosmetics low dose, enhance face
The moisturizing moisturizing in portion and barrier function.
2, in short-term in heat treatment process, 60 ± 5 DEG C of hot steam processing will not make the excessive thermal expansion pore of raw material, thermal sensitivity object
Matter, protein, vitamin are also unlikely to heated denaturalization, reduce remaining water content, and being cooled to room temperature rear active constituent will not
Inactivation；In freezing dry process, raw material can be frozen into solid, then come out steam sublimation under vacuum conditions, heat
Quick property substance, protein, vitamin isoreactivity substance can be left in the ice shelf freezed, it is dry after volume difference it is small, present
Loose porous structure, and oxygen is few under low temperature, is easy the phenolic substances being oxidized by oxygen, N- ester acyl sphingosine class object
Matter will not be oxidized inactivation, remain active material to the maximum extent.In crushing process, the flavones of non-refractory can be retained
The bioactive ingredients such as class, glycoside, carbohydrate, volatile oil sufficiently crush broken wall to the cell of Chinese medicine, promote releasing for active constituent
It puts and dissolves out, increase specific surface area, improve bioavilability.
3, it extracts in concentration process, is first extracted using the ethyl alcohol of large dosage of low concentration, reuse low dose of high concentration
Ethyl alcohol extract；On the one hand, the leaf skin mixing fine powders of small particle are pulverizing the abundant broken wall of process, effective component
It discharges substantially, carries out alcohol extracting without a large amount of high concentration ethanol；On the other hand, the contact area of low-concentration ethanol and fine powder
Greatly, Alcohol soluble composition recovery rate is high, reuses high concentration ethanol, supplements the ethyl alcohol evaporated, increases concentration of alcohol, extracts
The poor active material of alcohol-soluble, after the concentration of two step extracting solutions, the high blending constituent of available activity substance content.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, all other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1
A kind of preparation method of ceramide promotor, comprising the following steps:
1) raw material choose and pretreatment: in parts by weight, weigh 106 parts of pineapple leaves, 16 parts of Radix Paeoniae Alba, 23 parts of motherwort,
8 parts of oolong tea；Wherein, pineapple leaves are selected from growth two months or more 1 year, immature pineapple, stand and drain the water after pretreatment
Point；Radix Paeoniae Alba, motherwort, oolong tea are robbed water and are cleaned, and are dried for standby；Wherein, pineapple leaves pre-process specifically: cut into 1-3cm long
Strip infiltrates 25min using the sodium carbonate liquor of 6wt%, is put into the ultrasonic cleaner for be loaded with purified water and surpasses after taking-up
Sonication 7min.
2) it is heat-treated in short-term: pretreated pineapple leaves, Radix Paeoniae Alba, motherwort, oolong tea is sent into steam rotary dryer
In, it is passed through 62 DEG C of hot steam processing 4min, cooled to room temperature；
3) be freeze-dried, crush: pineapple leaves, Radix Paeoniae Alba, motherwort, oolong tea are sent into vacuum freeze drier, at -8 DEG C
It is freeze-dried 1.8h；Pulverizer precomminution is put into graininess, crosses 20-40 mesh, removes fine powder, ultramicro grinding obtains grain
8-12 μm of diameter of mixing fine powders；Wherein, it pulverizes and uses airslide disintegrating mill, grinding tolerance is 6-10m3/ min, air pressure
For 0.7-1.0MPa, tappered rating 5.5kW.
4) extract concentration: mixing fine powders are added in multi-function extractor, and 8 times of 75% ethyl alcohol of amount, refluxing extraction is added
1.6h adds 4 times of 85% ethyl alcohol of amount, refluxing extraction 50min, combined extract；Extracting solution vacuum suck single-effect external circulation is dense
In contracting tank, it is concentrated under reduced pressure and removes 3/4 ethyl alcohol, filtrate and filter residue is obtained by filtration；Wherein, when reduced pressure vacuum degree be -0.08~-
0.05MPa, temperature are 45-52 DEG C, steam pressure 0.08-0.12MPa.
5) filter residue extracts again: the filter residue of step 4) being added to the water of 10 times of amounts, is stirred evenly, 6 times of amount petroleum are successively used
Ether carries out single extraction, and 4 times of amount ethyl acetate carry out reextraction, and 4 times of amount ethyl alcohol are extracted three times；Collect reextraction and
The oily phase extracted three times, is concentrated under reduced pressure, and 0.5 μm of nanofiltration membrane obtains pale tan oil；Wherein, it is carried out when single extraction
The centrifuge separation of 1.6min carries out the centrifuge separation of 55s when reextraction, and the centrifuge separation of 28s is carried out when extracting three times.
6) auxiliary material adds: the pale tan oil of the filtrate of step 4), step 5) being mixed, concentration removes ethyl alcohol and mixed
Object A is closed, mixture A is uniformly mixed with suitable azone, menthol, cubeb oil.Wherein, azone, thin
Lotus alcohol, cubeb oil dosage be respectively 3%, 5%, the 7% of mixture A mass.
Embodiment 2
A kind of preparation method of ceramide promotor, comprising the following steps:
1) raw material is chosen and is pre-processed: in parts by weight, weighing 96 parts of pineapple leaves, 15 parts of Radix Paeoniae Alba, 26 parts of motherwort, crow
9 parts of imperial tea；Wherein, pineapple leaves are selected from growth two months or more 1 year, immature pineapple, stand and drain away the water after pretreatment；
Radix Paeoniae Alba, motherwort, oolong tea are robbed water and are cleaned, and are dried for standby；Wherein, pineapple leaves pre-process specifically: cut into 1-3cm strip
Shape infiltrates 22min using the sodium carbonate liquor of 8wt%, is put into the ultrasonic cleaner for be loaded with purified water after taking-up ultrasonic
Handle 6min.
2) it is heat-treated in short-term: pretreated pineapple leaves, Radix Paeoniae Alba, motherwort, oolong tea is sent into steam rotary dryer
In, it is passed through 60 ± 5 DEG C of hot steam processing 3-5min, cooled to room temperature；
3) be freeze-dried, crush: pineapple leaves, Radix Paeoniae Alba, motherwort, oolong tea are sent into vacuum freeze drier, at -10 DEG C
~-5 DEG C of freeze-drying 1-2h；Pulverizer precomminution is put into graininess, 20-40 mesh is crossed, removes fine powder, pulverize
Obtain 8-12 μm of partial size of mixing fine powders；Wherein, it pulverizes and uses airslide disintegrating mill, grinding tolerance is 6-10m3/ min, it is empty
Atmospheric pressure is 0.7-1.0MPa, tappered rating 5.5kW.
4) extract concentration: mixing fine powders are added in multi-function extractor, and 8 times of 75% ethyl alcohol of amount, refluxing extraction is added
1.8h adds 4 times of 85% ethyl alcohol of amount, refluxing extraction 52min, combined extract；Extracting solution vacuum suck single-effect external circulation is dense
In contracting tank, it is concentrated under reduced pressure and removes 3/4 ethyl alcohol, filtrate and filter residue is obtained by filtration；Wherein, when reduced pressure vacuum degree be -0.08~-
0.05MPa, temperature are 45-52 DEG C, steam pressure 0.08-0.12MPa.
5) filter residue extracts again: the filter residue of step 4) being added to the water of 10 times of amounts, is stirred evenly, 6 times of amount petroleum are successively used
Ether carries out single extraction, and 4 times of amount ethyl acetate carry out reextraction, and 4 times of amount ethyl alcohol are extracted three times；Collect reextraction and
The oily phase extracted three times, is concentrated under reduced pressure, and 0.5 μm of nanofiltration membrane obtains pale tan oil；Wherein, it is carried out when single extraction
The centrifuge separation of 1.5min carries out the centrifuge separation of 48s when reextraction, and the centrifuge separation of 26s is carried out when extracting three times.
6) auxiliary material adds: the pale tan oil of the filtrate of step 4), step 5) being mixed, concentration removes ethyl alcohol and mixed
Object A is closed, mixture A is uniformly mixed with suitable azone, menthol, cubeb oil.Wherein, azone, thin
Lotus alcohol, cubeb oil dosage be respectively 3-5%, 4-6%, 6-8% of mixture A mass.
Embodiment 3
A kind of preparation method of ceramide promotor, comprising the following steps:
1) raw material choose and pretreatment: in parts by weight, weigh 115 parts of pineapple leaves, 18 parts of Radix Paeoniae Alba, 27 parts of motherwort,
10 parts of oolong tea；Wherein, pineapple leaves are selected from growth two months or more 1 year, immature pineapple, stand and drain the water after pretreatment
Point；Radix Paeoniae Alba, motherwort, oolong tea are robbed water and are cleaned, and are dried for standby；Wherein, pineapple leaves pre-process specifically: cut into 1-3cm long
Strip infiltrates 30min using the sodium carbonate liquor of 6wt%, is put into the ultrasonic cleaner for be loaded with purified water and surpasses after taking-up
Sonication 8min.
2) it is heat-treated in short-term: pretreated pineapple leaves, Radix Paeoniae Alba, motherwort, oolong tea is sent into steam rotary dryer
In, it is passed through 65 DEG C of hot steam processing 3min, cooled to room temperature；
3) be freeze-dried, crush: pineapple leaves, Radix Paeoniae Alba, motherwort, oolong tea are sent into vacuum freeze drier, at -10 DEG C
~-5 DEG C of freeze-drying 1-2h；Pulverizer precomminution is put into graininess, 20-40 mesh is crossed, removes fine powder, pulverize
Obtain 8-12 μm of partial size of mixing fine powders；Wherein, it pulverizes and uses airslide disintegrating mill, grinding tolerance is 6-10m3/ min, it is empty
Atmospheric pressure is 0.7-1.0MPa, tappered rating 5.5kW.
4) extract concentration: mixing fine powders are added in multi-function extractor, and 8 times of 75% ethyl alcohol of amount, refluxing extraction 1- is added
2h adds 4 times of 85% ethyl alcohol of amount, refluxing extraction 40-60min, combined extract；Extracting solution vacuum suck single-effect external circulation is dense
In contracting tank, it is concentrated under reduced pressure and removes 3/4 ethyl alcohol, filtrate and filter residue is obtained by filtration；Wherein, when reduced pressure vacuum degree be -0.08~-
0.05MPa, temperature are 45-52 DEG C, steam pressure 0.08-0.12MPa.
5) filter residue extracts again: the filter residue of step 4) being added to the water of 10 times of amounts, is stirred evenly, 6 times of amount petroleum are successively used
Ether carries out single extraction, and 4 times of amount ethyl acetate carry out reextraction, and 4 times of amount ethyl alcohol are extracted three times；Collect reextraction and
The oily phase extracted three times, is concentrated under reduced pressure, and 0.5 μm of nanofiltration membrane obtains pale tan oil；Wherein, it is carried out when single extraction
The centrifuge separation of 1-2min carries out the centrifuge separation of 40-60s when reextraction, and the centrifugation point of 20-30s is carried out when extracting three times
From.
6) auxiliary material adds: the pale tan oil of the filtrate of step 4), step 5) being mixed, concentration removes ethyl alcohol and mixed
Object A is closed, mixture A is uniformly mixed with suitable azone, menthol, cubeb oil.Wherein, azone, thin
Lotus alcohol, cubeb oil dosage be respectively 3-5%, 4-6%, 6-8% of mixture A mass.
Comparative example 1
It is dried in 45-50 DEG C to aqueous the difference from embodiment 1 is that step 3) freeze-drying is replaced with using drying box
Amount is less than 5%.
Comparative example 2
The difference from embodiment 1 is that cancellation step 5) filter residue extracts again.
Comparative example 3
The difference from embodiment 1 is that step 6) is not added with azone.
Ceramide promotes experiment
1, Normal human epidermal's keratinocyte condition of culture: is sowed in EpiLife-KG2 (KURABO company) 6 orifice plates
(NHEK (F)), culture is to as aggregation (confluent) state.Hereafter be transformed to EpiLife-KG2 (addition of no proliferation because
Son), 2 microgram of ceramide promotor of above-described embodiment 1-3, comparative example 1-3 preparation is added respectively, and control group uses 10% second
Alcohol after culture 3 days, recycles cell from each hole.
2, lipids extraction: lipid is extracted from the cell of recycling by Bligh and Dyer method.Extracting solution is subjected to nitrogen
After drying, object is redissolved in chloroform/methanol mixed liquor and is made as lipid samples.Albumen quality is quantified by BCA method.
3, ceramide amount parses: being parsed in the lipid of extraction with thin-layer chromatography (TLC) method.With chloroform: methanol:
Acetic acid=190:9:1 horizontal direction is unfolded 2 times, dries up and sprays copper sulphate chromophoric solution, is toasted with heating plate and detect neural acyl
Amine, resulting value are divided by obtain ceramide amount with respective protein content.Specific experiment the results are shown in Table 1.Wherein, numerical value is with control group
Ceramide amount be 1 when relative value.
1. ceramide magnitude of table
As can be seen from the above table, the ceramide promotor of the embodiment of the present invention is after the parsing of lipid, ceramide amount
Value is high, illustrates that generating ceramide to Normal human epidermal's keratinocyte has good facilitation.Comparative example 1 is due to using normal
The heat drying of rule, is easy the phenolic substances being oxidized by oxygen, N- ester acyl sphingosine substance can be oxidized inactivation, causes to have
Effective component content reduces, the decline of ceramide facilitation.Comparative example 2 is extracted again due to lacking filter residue, there is the work of high level
Property remain in filter residue at branch, cause the recovery rate of raw material to reduce, facilitation decline.Comparative example 3 is due to lacking transdermal enhancer
Azone, so that promoting the effect of Transdermal absorption reduces.
Improve face wrinkles' experiment
Selection face wrinkles are obvious, dry skin is withered and yellow, and the age, the women of no skin allergy history volunteered between 40-60
60 people of person, every group of 20 people, the ceramide promotor prepared using embodiment 1-3 are applied to the canthus week for being easy to produce wrinkle
Side and forehead position, sooner or later respectively using primary, 15 days courses for the treatment of.The canthus of coating front and back is measured using two dimensional image analytic method
Small wrinkle, the small wrinkle rate of statistical average and small wrinkle improvement rate.Wherein, two dimensional image analytic method referring to [military field gram he supervize
Cosmetics serviceability-assessment technique progress and in the future prospect Yao Shi newspaper office p170 (2001)].Concrete outcome is shown in Table 2.
2. face wrinkles of table improve result
As can be seen from the above table, the ceramide promotor of preparation of the embodiment of the present invention is aobvious to face wrinkles' effect is improved
It writes, is suitble to promote the use of.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
Above content is only citing made for the present invention and explanation, affiliated those skilled in the art are to being retouched
The specific embodiment stated does various modifications or additions or is substituted in a similar manner, and without departing from invention or surpasses
More range defined in the claims, is within the scope of protection of the invention.
Claims (7)
1. a kind of preparation method of ceramide promotor, which comprises the following steps:
1) raw material is chosen and is pre-processed: in parts by weight, weighing 80-120 parts of pineapple leaves, 12-18 parts of Radix Paeoniae Alba, motherwort 20-
28 parts, 5-11 parts of oolong tea；Wherein, pineapple leaves are selected from growth two months or more 1 year, immature pineapple, stand after pretreatment
It drains away the water；Radix Paeoniae Alba, motherwort, oolong tea are robbed water and are cleaned, and are dried for standby；
2) it is heat-treated in short-term: pretreated pineapple leaves, Radix Paeoniae Alba, motherwort, oolong tea being sent into steam rotary dryer, led to
Enter 60 ± 5 DEG C of hot steam processing 3-5min, cooled to room temperature；
3) be freeze-dried, crush: pineapple leaves, Radix Paeoniae Alba, motherwort, oolong tea are sent into vacuum freeze drier, -10 DEG C~-5
DEG C freeze-drying 1-2h；Pulverizer precomminution is put into graininess, 20-40 mesh is crossed, removes fine powder, ultramicro grinding obtains
8-12 μm of partial size of mixing fine powders；
4) extract concentration: mixing fine powders are added in multi-function extractor, are added 8 times of 75% ethyl alcohol of amount, refluxing extraction 1-2h, then
4 times of 85% ethyl alcohol of amount, refluxing extraction 40-60min, combined extract is added；Extracting solution vacuum suck single-effect external circulation concentration tank
It is interior, it is concentrated under reduced pressure and removes 3/4 ethyl alcohol, filtrate and filter residue is obtained by filtration；
5) filter residue extracts again: the filter residue of step 4) is added to the water of 10 times of amounts, is stirred evenly, successively using 6 times of amount petroleum ethers into
Row single extraction, 4 times of amount ethyl acetate carry out reextraction, and 4 times of amount ethyl alcohol are extracted three times；Collect reextraction and three times
The oily phase of extraction, is concentrated under reduced pressure, and 0.5 μm of nanofiltration membrane obtains pale tan oil；
6) auxiliary material adds: the pale tan oil of the filtrate of step 4), step 5) being mixed, concentration removes ethyl alcohol and obtains mixture
Mixture A is uniformly mixed by A with suitable azone, menthol, cubeb oil.
2. the preparation method of ceramide promotor according to claim 1, which is characterized in that the step 1) pineapple leaves
Pretreatment specifically: cut into 1-3cm strip, infiltrate 20-30min using the sodium carbonate liquor of 6-8wt%, be put into after taking-up
It is loaded in the ultrasonic cleaner of purified water and is ultrasonically treated 5-8min.
3. the preparation method of ceramide promotor according to claim 1, which is characterized in that the step 3) Ultramicro-powder
Broken to use airslide disintegrating mill, grinding tolerance is 6-10m3/ min, air pressure 0.7-1.0MPa, tappered rating 5.5kW.
4. the preparation method of ceramide promotor according to claim 1, which is characterized in that the step 4) decompression is dense
Vacuum degree is -0.08~-0.05MPa when contracting, and temperature is 45-52 DEG C, steam pressure 0.08-0.12MPa.
5. the preparation method of ceramide promotor according to claim 1, which is characterized in that the step 5) once extracts
The centrifuge separation that 1-2min is carried out when taking, the centrifuge separation of 40-60s is carried out when reextraction, carries out 20-30s when extracting three times
Centrifuge separation.
6. the preparation method of ceramide promotor according to claim 1, which is characterized in that step 6) the laurel nitrogen
Ketone, menthol, cubeb oil dosage be respectively 3-5%, 4-6%, 6-8% of mixture A mass.
7. a kind of application of ceramide promotor, which is characterized in that the ceramide promotor is on improving face wrinkles
Using.
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