CN106420521A - Anoectochilus roxburghiiv flavone extraction process and application thereof in skin care products - Google Patents
Anoectochilus roxburghiiv flavone extraction process and application thereof in skin care products Download PDFInfo
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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
- A61K8/96—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
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- A61K8/00—Cosmetics or similar toiletry preparations
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- 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
- A61K8/4973—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
- A61K8/498—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom having 6-membered rings or their condensed derivatives, e.g. coumarin
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- A—HUMAN NECESSITIES
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- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
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- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
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- A61K2800/782—Enzyme inhibitors; Enzyme antagonists
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- 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
- A61K2800/82—Preparation or application process involves sonication or ultrasonication
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- 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 relates to an anoectochilus roxburghii flavone extraction process and application thereof in skin care products. The extraction process comprises the following steps of S1, conducting pulping, freeze drying and smashing on the anoectochilus roxburghii in sequence, and conducting extraction on the smashed anoectochilus roxburghii powder to obtain an anoectochilus roxburghii flavone crude extract liquid; S2, filtering the crude extract liquid obtained in the S1, reducing pressure and concentrating to obtain an anoectochilus roxburghii flavone crude extract; S3, conducting purification on the anoectochilus roxburghii flavone crude extract by adopting a Sephadex LH-20 gel column, so that an anoectochilus roxburghii flavone extract is obtained, wherein technological conditions in the S1 for freeze drying is a freezing temperature of 70-80 DEG C, freezing time of 40-60 hours and vacuum pressure of 15-25Pa. The provided extraction technology has high an extraction rate, and the anoectochilus roxburghii flavone extract obtained by extraction has high content of effective constituents, less impurities, and good antioxidant activity and tyrosinase activity inhibition.
Description
Technical field
The present invention relates to the extraction process of flavones, be specifically related to the extraction process of a kind of roxburgh anoectochilus terminal bud flavones and produce in skin care
Application in product.
Background technology
Roxburgh anoectochilus terminal bud [Anoecwchilus roxburghii (Wall.) Lindl] is the orchid family Anoectochilus Blume plant, which is many
Year raw Valuable Herbal Medicine, have another name called Shorthairy Antenoron, Anoectochilus Roxburghii, gold thread taiwan anetochilus herb, gold thread disappear to the marrow, gold silkworm, metal and stone pine, tree grass
Lotus, money grass etc..Roxburgh anoectochilus terminal bud herb all can be used as medicine, and taste is sweet, property is flat has the work(such as clearing heat and cooling blood, removing dampness and detoxicating, pain relieving, antibechic
Effect, is used for treating pulmonary tuberculosis, cough, rheumatic arthritis, traumatic injury, chronic gastritis, hepatitis, ephritis, cystitis clinically
Deng disease；Among the people for treating the pain such as acute nephritis, child convulsion and wind-cold-dampness arthralgia, and curative effect is especially pronounced, enjoy " king of medicine ",
The laudatory title such as " gold grass ", " crow ginseng ".The main active of roxburgh anoectochilus terminal bud is flavonoids, many glucides class, esters, sterol, life
The compositions such as alkaloids, triterpenes, trace element, have multiple physiologically active.Chromocor compound in roxburgh anoectochilus terminal bud, can be by effectively clearly
Except internal oxygen radical, stop degeneration, the aging of cell, thus there is raising body immunity, inhibition cancer cell growth
With prevent the effects such as hepatic injury.
The extraction process of current roxburgh anoectochilus terminal bud flavones mainly uses macroreticular resin initial gross separation method of purification and solvent extraction method.Greatly
Hole resin initial gross separation method of purification is time-consumingly long and recovery rate is low, and solvent extraction rule needs in substantial amounts of solvent and extract
Impurity content is higher；In addition, existing extraction process extracts the active constituent content in the roxburgh anoectochilus terminal bud chromocor extract obtaining relatively
Low.Roxburgh anoectochilus terminal bud is one of exclusive Chinese herbal medicine of China, and therefore the research of the extraction technology of preparing of roxburgh anoectochilus terminal bud flavones is to abundant exploitation
Roxburgh anoectochilus terminal bud resource is significant.
For the deficiency of existing roxburgh anoectochilus terminal bud extracting flavonoids technique, it is desirable to provide a kind of recovery rate is high, gained extracts
The extraction process of the roxburgh anoectochilus terminal bud flavones that in thing, active constituent content is high, impurity is few.
Content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, the extraction process of a kind of roxburgh anoectochilus terminal bud flavones is provided, this
The extraction process of bright offer has higher recovery rate；Active constituent content in gained roxburgh anoectochilus terminal bud chromocor extract is high, impurity
Few, there is preferable antioxidation activity and suppression tyrosinase activity.
Another object of the present invention is to provide application in skin-protection product for the roxburgh anoectochilus terminal bud.
For achieving the above object, the present invention adopts the following technical scheme that：
The extraction process of a kind of roxburgh anoectochilus terminal bud flavones, described extraction process comprises the steps：
S1：Roxburgh anoectochilus terminal bud is pulled an oar successively, freeze-drying, pulverizing, to pulverize after roxburgh anoectochilus terminal bud powder carry out extracting to obtain gold thread
Lotus flavones crude extract；
S2：Filter S1 gained crude extract, reduced pressure concentration obtains roxburgh anoectochilus terminal bud flavones crude extract；
S3：Use Sephadex LH-20 gel column to be purified roxburgh anoectochilus terminal bud flavones crude extract i.e. to obtain roxburgh anoectochilus terminal bud flavones and carry
Take thing；
Wherein, cryodesiccated process conditions described in S1 be cryogenic temperature-70 DEG C～-80 DEG C, cooling time 40h～
60h, Vacuum Pressure 15Pa～25Pa.
Not being destroyed for the functional component in maximum protection roxburgh anoectochilus terminal bud, the present invention selects at Freeze Drying Technique
Reason roxburgh anoectochilus terminal bud, inventor find the cryogenic temperature in Freeze Drying Technique and vacuum to the extraction of active ingredient in roxburgh anoectochilus terminal bud and
The impact of recovery rate is relatively big, when cryodesiccated process conditions be cryogenic temperature-70 DEG C～-80 DEG C, cooling time 40h～60h,
During Vacuum Pressure 15Pa～25Pa, the roxburgh anoectochilus terminal bud after freeze-drying is processed not only has higher recovery rate, is extracted the gold obtaining
Line lotus chromocor extract also has higher antioxidation activity and suppression tyrosinase activity.In the present invention, vacuum is too low
The water sublimed in roxburgh anoectochilus terminal bud can be made not thorough, and effect is poor, and vacuum is too high then high to instrument requirements, and energy consumption is greatly simultaneously
The service life of instrument can be shortened；The too high meeting of cryogenic temperature causes roxburgh anoectochilus terminal bud sample freezing not thorough, and drying effect is poor；Separately
Outward, cryogenic temperature is too high or too low all can have to instrument compared with lossy, and the too low meeting of cryogenic temperature causes energy consumption to raise.
The present inventor also attempts various method to remove the impurity in gained roxburgh anoectochilus terminal bud flavones crude extract, Jing Guozhong
Inventor's discovery after many trials, can be when selecting Sephadex LH-20 gel column to purify roxburgh anoectochilus terminal bud flavones crude extract
The impurity removing in crude extract of limits, and it is enriched with the content of roxburgh anoectochilus terminal bud flavones, use Sephadex LH-20 gel column pure
The flavones content changed in the roxburgh anoectochilus terminal bud chromocor extract obtaining is up to 60～90%；And select Sephadex LH-20 gel column
Purification time short, and select the disengaging time length of other gel columns and separating effect not good.
The present invention extracts after carrying out freeze-drying to roxburgh anoectochilus terminal bud again, and extract is after filtration, reduced pressure concentration, then uses
Sephadex LH-20 gel column purifies, and the active constituent content in the Anoectochilus obtaining is high, impurity is few, has preferably
Antioxidant effect and suppression tyrosinase activity.
Preferably, cryodesiccated process conditions described in S1 are cryogenic temperature-78 DEG C, cooling time 48h, Vacuum Pressure
20Pa.
Preferably, the extracting mode in S1 is water-bath extraction, ultrasonic extraction or Microwave Extraction.
The theoretical foundation that ultrasonic wave extracts is to utilize ultrasonic wave calorifics mechanism, ultra sonic machinery mechanism and cavitation, makes
Plant cell wall ruptures and is discharged into target product in extract.Ultrasonic wave extract carry with water-bath, compared with Microwave Extraction, it carries
Taking speed faster, treating capacity is higher, and the impurity in extract is low compared with conventional method.It is preferred that the extracting mode in S1
For ultrasonic extraction.
In we's invention, the technique of preferably described ultrasonic extraction is：Ultrasonic power 400～800W, concentration of alcohol 50
～70%, solid-liquid ratio 1:100～200, extraction time 40～80min, Extracting temperature 50～60 DEG C.
For enable flavone compound in roxburgh anoectochilus terminal bud flavones crude extract and impurity more preferably, separate faster, at this
When bright S3 using Sephadex LH-20 gel column be purified, the volume of roxburgh anoectochilus terminal bud crude extract and the volume ratio of gel column
It is 1：15～1：25；It is further preferable that the volume of roxburgh anoectochilus terminal bud crude extract is 1 with the volume ratio of gel column：20.
Preferably, S3 use volume fraction be that the ethanol solution of 30～90% is as eluent；Use ethanol as washing
De-liquid, can avoid other organic solvents to target product obtaining the higher roxburgh anoectochilus terminal bud chromocor compound of purity simultaneously to greatest extent
Pollution, it is ensured that it uses the security of cosmetics.It is further preferable that the ethanol solution using volume fraction to be 90% is made
For eluent.
It is better that the post footpath of Sephadex LH-20 gel column and the ratio of post height are essentially higher separating effect, but at this
If ratio exceeds 1 in bright:80 flow velocitys are excessively slow, affect the efficiency of separation and Extraction, and when the ratio in post footpath and post height is less than 1:50
Shi Zehui causes and cannot be sufficiently separated impurity；During it is preferred that S3 uses Sephadex LH-20 gel column be purified,
The post footpath volume ratio high with post is 1:40～1:60；It is further preferable that the post footpath volume ratio high with post is 1:50.
Preferably, when using Sephadex LH-20 gel column to be purified in S3, flow velocity is 1.0ml/min.
Preferably, it is filtered into described in S2 and takes out under conditions of being 15～20um double-layer filter paper in-0.1MPa vacuum, aperture
Filter.
Preferably, reduced pressure concentration described in S2 is for being 115rpm/min in-0.1MPa vacuum, rotary speed, evaporating temperature
45 DEG C, concentrate under conditions of circulating condensing temperature 2 DEG C.
Another object of the present invention is to provide roxburgh anoectochilus terminal bud chromocor extract as NMF or whitening agent at skin-protection product
In application.
Compared with prior art, the present invention has the advantages that：
(1) present invention can farthest protect active ingredient in roxburgh anoectochilus terminal bud to extracting after roxburgh anoectochilus terminal bud freeze-drying again
And improving the recovery rate of roxburgh anoectochilus terminal bud flavones, recovery rate can reach more than 2.5%, makes the roxburgh anoectochilus terminal bud chromocor extract tool finally giving
Have preferable antioxidation activity and suppression tyrosinase activity；
(2) present invention uses Sephadex LH-20 gel column to be purified roxburgh anoectochilus terminal bud crude extract, farthest removes
Remove the impurity in crude extract, roxburgh anoectochilus terminal bud flavones content in Sync enrichment extract；
(3) extraction process that the present invention provides is compared with solvent extraction method and macroreticular resin separating and extracting process, the present invention
Extract flavones content in the roxburgh anoectochilus terminal bud chromocor extract that obtains higher and active by force, flavones content in gained Anoectochilus
Up to more than 75%.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.These embodiments are only that the typical case to the present invention retouches
State, but the invention is not restricted to this.Test method used in following embodiment if no special instructions, is conventional method, is made
Raw material, reagent etc., if no special instructions, be the raw material that can obtain from the routine commercial sources such as commercial and reagent.
Embodiment 1
(1) fresh roxburgh anoectochilus terminal bud is pulled an oar, at cryogenic temperature-78 DEG C, cooling time 48h, freezing under the conditions of Vacuum Pressure 20Pa
It is dried and pulverizes and to obtain roxburgh anoectochilus terminal bud powder；Weigh 3.00g roxburgh anoectochilus terminal bud powder, at ultrasonic power 600W, solid-liquid ratio 1：150, ethanol is dense
Degree 60%, extraction time is 60min, extracts, obtain roxburgh anoectochilus terminal bud flavones crude extract under conditions of Extracting temperature 60 DEG C；
(2) roxburgh anoectochilus terminal bud flavones crude extract is filtered under the conditions of-0.1MPa vacuum, aperture 15～20um double-layer filter paper,
Then vacuum, rotary speed 115rpm/min at-0.1MPa, evaporating temperature 45 DEG C, subtract under conditions of circulating condensing temperature 2 DEG C
Pressure is concentrated to give roxburgh anoectochilus terminal bud flavones crude extract；
(3) roxburgh anoectochilus terminal bud flavones CE being crossed Sephadex LH-20 gel column, gel column post footpath with the ratio of post height is
1:50, the volume of roxburgh anoectochilus terminal bud crude extract and the volume ratio of gel column are 1：20, the ethanol solution using volume fraction to be 60% is made
For eluent, elution flow rate is 1.0ml/min, elutes 2～3 column volumes, obtains roxburgh anoectochilus terminal bud chromocor extract, measures extract
Middle flavones content, anti-oxidant value and suppression TYR enzymatic activity.
Embodiment 2
(1) fresh roxburgh anoectochilus terminal bud is pulled an oar, at cryogenic temperature-70 DEG C, cooling time 40h, freezing under the conditions of Vacuum Pressure 15Pa
It is dried and pulverizes and to obtain roxburgh anoectochilus terminal bud powder；Weigh 3.00g roxburgh anoectochilus terminal bud powder, at microwave power 800W, solid-liquid ratio 1：100, ethanol is dense
Degree 50%, extraction time is 40min, extracts, obtain roxburgh anoectochilus terminal bud flavones crude extract under conditions of Extracting temperature 40 DEG C；
(2) roxburgh anoectochilus terminal bud flavones crude extract is filtered under the conditions of-0.1MPa vacuum, aperture 15～20um double-layer filter paper,
Then vacuum, rotary speed 115rpm/min at-0.1MPa, evaporating temperature 45 DEG C, subtract under conditions of circulating condensing temperature 2 DEG C
Pressure is concentrated to give roxburgh anoectochilus terminal bud flavones crude extract；
(3) roxburgh anoectochilus terminal bud flavones CE being crossed Sephadex LH-20 gel column, gel column post footpath with the ratio of post height is
1:50, the volume of roxburgh anoectochilus terminal bud crude extract and the volume ratio of gel column are 1：15, the ethanol solution using volume fraction to be 70% is made
For eluent, elution flow rate is 1.0ml/min, elutes 2～3 column volumes, obtains roxburgh anoectochilus terminal bud chromocor extract, measures extract
Middle flavones content, anti-oxidant value and suppression TYR enzymatic activity.
Embodiment 3
(1) fresh roxburgh anoectochilus terminal bud is pulled an oar, at cryogenic temperature-80 DEG C, cooling time 60h, freezing under the conditions of Vacuum Pressure 25Pa
It is dried and pulverizes and to obtain roxburgh anoectochilus terminal bud powder；Weigh 3.00g roxburgh anoectochilus terminal bud powder, at microwave power 400W, solid-liquid ratio 1：200, ethanol is dense
Degree 60%, extraction time is 1200min, and water-bath under conditions of Extracting temperature 80 DEG C is extracted, and obtains roxburgh anoectochilus terminal bud flavones crude extract；
(2) roxburgh anoectochilus terminal bud flavones crude extract is filtered under the conditions of-0.1MPa vacuum, aperture 15～20um double-layer filter paper,
Then vacuum, rotary speed 115rpm/min at-0.1MPa, evaporating temperature 45 DEG C, subtract under conditions of circulating condensing temperature 2 DEG C
Pressure is concentrated to give roxburgh anoectochilus terminal bud flavones crude extract liquid；
(3) roxburgh anoectochilus terminal bud flavones CE being crossed Sephadex LH-20 gel column, gel column post footpath with the ratio of post height is
1:50, the volume of roxburgh anoectochilus terminal bud crude extract and the volume ratio of gel column are 1：25, the ethanol solution using volume fraction to be 90% is made
For eluent, elution flow rate is 1.0ml/min, elutes 2～3 column volumes, obtains roxburgh anoectochilus terminal bud chromocor extract, measures extract
Middle flavones content, anti-oxidant value and suppression TYR enzymatic activity.
Embodiment 4
(1) fresh roxburgh anoectochilus terminal bud is pulled an oar, at cryogenic temperature-80 DEG C, cooling time 60h, freezing under the conditions of Vacuum Pressure 25Pa
It is dried and pulverizes and to obtain roxburgh anoectochilus terminal bud powder；Weigh 3.29g roxburgh anoectochilus terminal bud and dry sample, at ultrasonic power 500W, solid-liquid ratio 1：120, ethanol
Concentration 55%, extracts under conditions of extraction time is 100min, Extracting temperature 50 DEG C, obtains roxburgh anoectochilus terminal bud flavones crude extract；
(2) roxburgh anoectochilus terminal bud flavones crude extract is filtered under the conditions of-0.1MPa vacuum, aperture 15～20um double-layer filter paper,
Then vacuum, rotary speed 115rpm/min at-0.1MPa, evaporating temperature 45 DEG C, subtract under conditions of circulating condensing temperature 2 DEG C
Pressure is concentrated to give roxburgh anoectochilus terminal bud flavones crude extract；
(3) roxburgh anoectochilus terminal bud flavones CE being crossed Sephadex LH-20 gel column, gel column post footpath with the ratio of post height is
1:50, the volume of roxburgh anoectochilus terminal bud crude extract and the volume ratio of gel column are 1：18, the ethanol solution using volume fraction to be 80% is made
For eluent, elution flow rate is 1.0ml/min, elutes 2～3 column volumes, obtains roxburgh anoectochilus terminal bud chromocor extract, measures extract
Middle flavones content, anti-oxidant value and suppression TYR enzymatic activity.
Reference examples 1
In this reference examples after roxburgh anoectochilus terminal bud is directly pulled an oar by step (1) i.e. ultrasonic extract in addition to, other techniques with
Embodiment 1 is identical.
(1) pulling an oar fresh roxburgh anoectochilus terminal bud, taking 59.52g slurries, add 95% ethanol 284.21ml, water 106.27ml, stirring is all
Even, at ultrasonic power 600W, solid-liquid ratio 1：150, concentration of alcohol 60%, extracts under conditions of extraction time 60min, obtains roxburgh anoectochilus terminal bud
Flavones crude extract；
(2) roxburgh anoectochilus terminal bud flavones crude extract is filtered under the conditions of-0.1MPa vacuum, aperture 15～20um double-layer filter paper,
Then vacuum, rotary speed 115rpm/min at-0.1MPa, evaporating temperature 45 DEG C, subtract under conditions of circulating condensing temperature 2 DEG C
Pressure is concentrated to give roxburgh anoectochilus terminal bud flavones crude extract；
(3) roxburgh anoectochilus terminal bud flavones CE being crossed Sephadex LH-20 gel column, gel column post footpath with the ratio of post height is
1:50, the volume of roxburgh anoectochilus terminal bud crude extract and the volume ratio of gel column are 1：20, the ethanol solution using volume fraction to be 60% is made
It is 1.0ml/min for elution flow velocity, elutes 2～3 column volumes, obtain roxburgh anoectochilus terminal bud chromocor extract, measure extract
Middle flavones content, anti-oxidant value and suppression TYR enzymatic activity.
Reference examples 2
In this reference examples in addition to selecting oven drying roxburgh anoectochilus terminal bud in step (1), other techniques are same as in Example 1.
(1) fresh roxburgh anoectochilus terminal bud being put into 60 DEG C of baking ovens and drying 72h, obtaining water content is 8.75% roxburgh anoectochilus terminal bud dry sample, high speed powder
Broken machine is pulverized, and weighs 3.29g roxburgh anoectochilus terminal bud dry sample powder, at ultrasonic power 600W, solid-liquid ratio 1：150, concentration of alcohol 60%, carry
Extract under conditions of taking time 60min, obtain roxburgh anoectochilus terminal bud flavones crude extract；
(2) roxburgh anoectochilus terminal bud flavones crude extract is filtered under the conditions of-0.1MPa vacuum, aperture 15～20um double-layer filter paper,
Then vacuum, rotary speed 115rpm/min at-0.1MPa, evaporating temperature 45 DEG C, subtract under conditions of circulating condensing temperature 2 DEG C
Pressure is concentrated to give roxburgh anoectochilus terminal bud flavones crude extract；
(3) roxburgh anoectochilus terminal bud flavones CE being crossed Sephadex LH-20 gel column, gel column post footpath with the ratio of post height is
1:50, the volume of roxburgh anoectochilus terminal bud crude extract and the volume ratio of gel column are 1：20, the ethanol solution using volume fraction to be 60% is made
For eluent, elution flow rate is 1.0ml/min, elutes 2～3 column volumes, obtains roxburgh anoectochilus terminal bud chromocor extract, measures extract
Middle flavones content, anti-oxidant value and suppression TYR enzymatic activity.
Reference examples 3
In this reference examples except the cryogenic temperature in step (1) and Vacuum Pressure different from embodiment 1 in addition to, other techniques with
Embodiment 1 is identical.
(1) fresh roxburgh anoectochilus terminal bud is pulled an oar, at cryogenic temperature-58 DEG C, cooling time 48h, freezing under the conditions of Vacuum Pressure 10Pa
It is dried and pulverizes and to obtain roxburgh anoectochilus terminal bud powder；Weigh 3.00g roxburgh anoectochilus terminal bud powder, at ultrasonic power 600W, solid-liquid ratio 1：150, ethanol is dense
Degree 60%, extraction time is 60min, extracts, obtain roxburgh anoectochilus terminal bud flavones crude extract under conditions of Extracting temperature 60 DEG C；
(2) roxburgh anoectochilus terminal bud flavones crude extract is filtered under the conditions of-0.1MPa vacuum, aperture 15～20um double-layer filter paper,
Then vacuum, rotary speed 115rpm/min at-0.1MPa, evaporating temperature 45 DEG C, subtract under conditions of circulating condensing temperature 2 DEG C
Pressure concentrates roxburgh anoectochilus terminal bud flavones crude extract；
(3) roxburgh anoectochilus terminal bud flavones CE being crossed Sephadex LH-20 gel column, gel column post footpath with the ratio of post height is
1:50, the volume of roxburgh anoectochilus terminal bud crude extract and the volume ratio of gel column are 1：20, the ethanol solution using volume fraction to be 60% is made
For eluent, elution flow rate is 1.0ml/min, elutes 2～3 column volumes, obtains roxburgh anoectochilus terminal bud chromocor extract, measures extract
Middle flavones content, anti-oxidant value and suppression TYR enzymatic activity.
Reference examples 4
In this reference examples except the cryogenic temperature in step (1) and Vacuum Pressure different from embodiment 1 in addition to, other techniques with
Embodiment 1 is identical.
(1) fresh roxburgh anoectochilus terminal bud is pulled an oar, at cryogenic temperature-88 DEG C, cooling time 48h, freezing under the conditions of Vacuum Pressure 30Pa
It is dried and pulverizes and to obtain roxburgh anoectochilus terminal bud powder；Weigh 3.00g roxburgh anoectochilus terminal bud powder, at ultrasonic power 600W, solid-liquid ratio 1：150, ethanol is dense
Degree 60%, extraction time is 60min, extracts, obtain roxburgh anoectochilus terminal bud flavones crude extract under conditions of Extracting temperature 60 DEG C；
(2) roxburgh anoectochilus terminal bud flavones crude extract is filtered under the conditions of-0.1MPa vacuum, aperture 15～20um double-layer filter paper,
Then vacuum, rotary speed 115rpm/min at-0.1MPa, evaporating temperature 45 DEG C, subtract under conditions of circulating condensing temperature 2 DEG C
Pressure is concentrated to give roxburgh anoectochilus terminal bud flavones crude extract；
(3) roxburgh anoectochilus terminal bud flavones CE being crossed Sephadex LH-20 gel column, gel column post footpath with the ratio of post height is
1:50, the volume of roxburgh anoectochilus terminal bud crude extract and the volume ratio of gel column are 1：20, the ethanol solution using volume fraction to be 60% is made
For eluent, elution flow rate is 1.0ml/min, elutes 2～3 column volumes, obtains roxburgh anoectochilus terminal bud chromocor extract, measures extract
Middle flavones content, anti-oxidant value and suppression TYR enzymatic activity.
Freeze-drying in the step (3) of embodiment 1～4 and reference examples 1～4 obtains flavones in roxburgh anoectochilus terminal bud chromocor extract and contains
The test result of amount, antioxidation activity and suppression TYR enzymatic activity see table 1.
(1) recovery rate
Recovery rate refers to that freeze-dried rear middle its flavones that measures of the roxburgh anoectochilus terminal bud chromocor extract obtaining in step (3) contains
The ratio of amount, flavones content and 3.00g roxburgh anoectochilus terminal bud powder is the recovery rate of roxburgh anoectochilus terminal bud.
(2) flavones content
The mensuration of flavones content uses colorimetric method, takes step (3) M afterwards1The roxburgh anoectochilus terminal bud chromocor extract of mg, adds distillation
Water is to V1Ml redissolves, and takes the sample solution 2ml after redissolution and mixes with 0.2ml 5%ml (w/v) sodium nitrite solution.After 6min,
Add 0.2ml 10%AlCl3·6H2O (w/v) solution, mixing shakes up.Add 2ml 1mol/L NaOH after 5min, treat anti-
Liquid is answered fully to be mixed.Measure absorbance at 510nm wavelength after 15min.Rutin uses above method to obtain as standard items
With sample concentration (c) to the equation of linear regression of absorbance (A) as A=1.650c-0.017 (r=0.999 6).According to rutin
Calibration curve calculates flavones content.
Wherein c is sample concentration after measurement, and V1 is sample volume after redissolution, and M1 is the roxburgh anoectochilus terminal bud extracting flavonoids material redissolving
Amount.
(3) antioxidation activity
1. DPPH clearance rate measures
Accurately weigh 20mgDPPH, by methanol constant volume to 500ml, obtain 0.04mg/ml mother liquor, take 0.2ml debita spissitudo sample
Product liquid, in 20ml test tube, adds 7.8ml above-mentioned DPPH solution, after reacting 30min under the conditions of lucifuge, under the conditions of 517nm
Survey light absorption value.The another DPPH gradient solution configuring variable concentrations, takes 8ml reaction assay under these conditions in 20ml test tube,
Obtain with sample introduction concentration (c) to the equation of linear regression of absorbance (A) as A=20.536c-0.0106 (r=0.999 9).Root
According to DPPH concentration in sample after calibration curve calculating reaction.Calculate the removing of DPPH in sample according to formula Y=(S-N)/S*100
Rate.(S is DPP concentration in blank sample, and N is DPPH concentration in sample.)
2. FRAP method surveys total antioxidation value
FRAP working solution matching while using：By the acetate buffer of 25ml 300mmol/L PH3.6,2.5ml10mmol/
LTPTZ solution, 2.5ml 20mmol/LFeCl3Solution mixes.
Draw the FeSO of certain gradient concentration respectively4Titer 0.1ml, adds 3mlFRAP working solution, adds 0.3ml
Ultra-pure water, is mixed, accurate response 5min, measures its light absorption value at 593nm, with ultra-pure water zeroing, draws calibration curve, by upper
Method of stating with sample introduction concentration (c) to the equation of linear regression of absorbance (A) as A=0.5975c+0.0311 (r=0.999 9).
The mensuration of sample：Measure the sample solution of 0.1ml, measure the total antioxidation value of sample in the above conditions.
The antioxidation activity (FRAP value) of sample is to reach FeSO needed for identical absorbance4A mM number represent.
3. the mensuration of reducing power
Oyaiaz method is used to measure the reducing power of sample：
0.5ml sample solution is separately added into 0.2mol/L phosphate buffer (pH6.6) 2.5ml and 1% potassium ferricyanide
Solution 2.5ml, mix be placed in 50 DEG C of water reaction 20min be subsequently adding 10% solution of trichloroacetic acid 2.5ml, 3000r/
Min centrifuges 10min, takes 2.5ml supernatant, is sequentially added into 2.5ml distilled water and 0.5ml0.1% liquor ferri trichloridi, fully mixed
Closing, 700nmchu measures the light absorption value of sample, and light absorption value is higher, and reducing power is stronger.
(4) tyrosinase activity is suppressed
It is pressed into the volume such as table 1 below with micropipettor respectively and accurately draw the TYR in T1, T2, T3, T4, PBS
The reactant liquor of buffer solution and sample is respectively placed in 4 PE pipes, mixes, 37 DEG C of constant temperature 10min, then adds respectively in T2, T4
Entering the tyrosinase of 1mL, reacting 10min, quick ultraviolet specrophotometer measures its absorbance A at 475nmT1、AT2、AT3、
AT4.Calculate the activity of sample suppression tyrosinase as follows：Inhibitory activity against tyrosinase=[1-(AT4-AT3)/(AT2-
AT1)] × 100% wherein, AT1：It is not loaded product and do not add the absorbance A that the reactant liquor of tyrosinase records at 475nmT2：Not
Sample-adding product add absorbance A at 475nm for the reactant liquor of tyrosinaseT3：Sample-adding product and the reactant liquor that do not adds tyrosinase exist
The absorbance A recording at 475nmT4：Sample-adding product and add the extinction that the reactant liquor of tyrosinase records at 475nm.
Table 1 reactant liquor forms
The performance test of the roxburgh anoectochilus terminal bud chromocor extract obtaining in table 2 embodiment 1～4 and reference examples 1～4
Application test example one
This application test example gives the emulsion of two kinds of formulas (wt%)：
Formula 1：Jojoba seed oil 8.0g, saualane 3.0g, glycerine 5.0g, propane diols 4.0g, hydrolecithin 2.0g, real
Execute example 1 and extract the roxburgh anoectochilus terminal bud chromocor extract 2.0g obtaining, card ripple U21 0.1g, triethanolamine 0.1g, add water to 100g；
Formula 2：Jojoba seed oil 8.0g, saualane 3.0g, glycerine 5.0g, propane diols 4.0g, hydrolecithin 2.0g, card
Ripple U21 0.1g, triethanolamine 0.1g, add water to 100g.
After selecting 30 trial volunteers respectively to use 2 months, simultaneously to fill a prescription 2 as compareing, to filling a prescription, 1 using effect is entered
The marking of row skin whitening, moisturizing is evaluated；Full marks are for very, and more than 8 points is excellent, and 6～8 are divided into well, and 3～6 are divided into typically, and less than 3 points are
To no effect, evaluation result such as table 3 below.
The skin whitening, moisturizing test of table 3 embodiment 1 gained roxburgh anoectochilus terminal bud chromocor extract
Application Example two
The performance of keeping humidity extracting the roxburgh anoectochilus terminal bud crude extract obtaining to embodiment 1～4 and reference examples 1～4 is tested, and with
Glycerine and hyaluronic acid are respectively as reference examples 5 and reference examples 6, and method of testing is as follows, and test result see table 2.
(1) hygroscopicity measures
Sample is placed in baking oven, at 105 DEG C, dries 3h, then place in silica gel drier and be cooled to room temperature.Accurate
Really weighing 1.0g, being respectively placed in and maintaining relative humidity (RH) with the saturated ammonium sulfate aqueous solution is 81%.Saturated calcium chloride water
Moisture absorption in the drier maintaining RH to be 32%, claims the quality of each sample after 24h, 72h.
Hydroscopicity (Ra)=(Wn-W0)/W0× 100%
W0For placing front sample quality, Wn is the sample quality after placement.
(2) moisture retention measures
The water adding mass fraction to be 10% in being dried the sample after constant weight, being then placed on RH is the 81%th, 32%
And in silica gel drier.The quality of each sample is claimed after 24h, 72h.
Moisturizing rate (Rr)=Hn/H0× 100%
H0For placing front biodiversity, Hn is biodiversity after placement.
Table, the test condition in 4 is：25 DEG C, relative humidity 32%；Test condition in table 5 is：25 DEG C, relative humidity
81%.
Table 4 embodiment 1～4 and reference examples 1～6 extract the performance of keeping humidity of the roxburgh anoectochilus terminal bud crude extract obtaining
Table 4 embodiment 1～4 and reference examples 1～6 extract the performance of keeping humidity of the roxburgh anoectochilus terminal bud crude extract obtaining
The 5th, table 6 be can be seen that various embodiments of the present invention extract the comprehensive performance of keeping humidity of the roxburgh anoectochilus terminal bud chromocor extract obtaining
All be better than each reference examples with moisture pick-up properties, roxburgh anoectochilus terminal bud chromocor extract can use making up as a kind of NMF, whitening agent
In product.
Claims (10)
1. the extraction process of a roxburgh anoectochilus terminal bud flavones, it is characterised in that described extraction process comprises the steps：
S1：Roxburgh anoectochilus terminal bud is pulled an oar successively, freeze-drying, pulverizing, carry out extracting that to obtain roxburgh anoectochilus terminal bud yellow to the roxburgh anoectochilus terminal bud powder after pulverizing
Ketone crude extract；
S2：Filter S1 gained crude extract, reduced pressure concentration obtains roxburgh anoectochilus terminal bud flavones crude extract；
S3：Use Sephadex LH-20 gel column to be purified roxburgh anoectochilus terminal bud flavones crude extract and i.e. obtain roxburgh anoectochilus terminal bud extracting flavonoids
Thing；
Wherein, cryodesiccated process conditions described in S1 are cryogenic temperature-70 DEG C～-80 DEG C, cooling time 40h～60h, true
Pneumatics 15Pa～25Pa.
2. the extraction process of roxburgh anoectochilus terminal bud flavones according to claim 1, it is characterised in that cryodesiccated technique described in S1
Condition is cryogenic temperature-78, cooling time 48h, Vacuum Pressure 20Pa.
3. the extraction process of roxburgh anoectochilus terminal bud flavones according to claim 1, it is characterised in that the extracting mode in S1 is that water-bath carries
Take, ultrasonic extract or Microwave Extraction.
4. the extraction process of roxburgh anoectochilus terminal bud flavones according to claim 3, it is characterised in that the extracting mode in S1 is ultrasonic carrying
Take.
5. the extraction process of roxburgh anoectochilus terminal bud flavones according to claim 4, it is characterised in that the technique of described ultrasonic extraction is：
Ultrasonic power 400～800W, concentration of alcohol 50～70%, solid-liquid ratio 1:100～200, extraction time 40～120min, extraction temperature
Spend 40～80 DEG C.
6. the extraction process of roxburgh anoectochilus terminal bud flavones according to claim 1, it is characterised in that use Sephadex LH-20 in S3
When gel column is purified, the volume of roxburgh anoectochilus terminal bud crude extract and the volume ratio of gel column are 1：15～1：25.
7. the extraction process of roxburgh anoectochilus terminal bud flavones according to claim 6, it is characterised in that use Sephadex LH-20 in S3
When gel column is purified, the volume of roxburgh anoectochilus terminal bud crude extract and the volume ratio of gel column are 1：20.
8. the extraction process of roxburgh anoectochilus terminal bud flavones according to claim 1, it is characterised in that use Sephadex LH-20 in S3
When gel column is purified, the post footpath volume ratio high with post is 1:40～1:60.
9. the extraction process of roxburgh anoectochilus terminal bud flavones according to claim 1, it is characterised in that be filtered into described in S2-
Suction filtration under conditions of 0.1MPa vacuum, aperture are 15～20um double-layer filter paper；Reduced pressure concentration described in S2 is true at-0.1MPa
Empty, rotary speed is 115rpm/min, and evaporating temperature 45 DEG C concentrates under conditions of circulating condensing temperature 2 DEG C.
10. roxburgh anoectochilus terminal bud chromocor extract application in skin-protection product as NMF or whitening agent.
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