CN104940049B - Extracting method, extract and the application of yacon plant extracts - Google Patents

Extracting method, extract and the application of yacon plant extracts Download PDF

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Publication number
CN104940049B
CN104940049B CN201410124593.2A CN201410124593A CN104940049B CN 104940049 B CN104940049 B CN 104940049B CN 201410124593 A CN201410124593 A CN 201410124593A CN 104940049 B CN104940049 B CN 104940049B
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yacon
plant extracts
ethanol water
mass percent
gradient elution
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CN104940049A (en
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文岳中
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention discloses a kind of extracting method of yacon plant extracts, including:In leaf or root tuber to pretreated yacon, ethanol or ethanol water are added as extractant, ultrasound, filtering, filtrate concentration;Concentrate is separated by macroporous resin column chromatography, column chromatography uses gradient elution, is first eluted with deionized water, and then with mass percent concentration, gradually increased ethanol water carries out gradient elution respectively successively, and post processing obtains extract.The invention also discloses the yacon plant extracts obtained by the above method and the application process of the extract.The present invention uses leaf or the root tuber of yacon as raw material, by simple extraction process, it can obtain the extract component with whitening function and anti-aging effect of different activities, can be according to being actually needed carry out categorised collection, and it is further prepared into required product, it is practical, there are wide market prospects.

Description

Extracting method, extract and the application of yacon plant extracts
Technical field
The invention belongs to technical field of plant extraction, be specifically related to a kind of extracting method of yacon plant extracts, Extract and as whitening active thing, anti-aging active thing and the application for including these whitening active things, anti-aging active thing.
Background technology
In the determinant of the colour of skin of people, the activity that human body produces the melanocyte of melanin occupies most important position Put.Research shows that human melanocyte produces melanin by the activity of various enzymes (for example, tyrosinase), melanin Forming process also by inherent cause, hormone secretion, with stress be relevant physiologic factor and environmental factor (for example, ultraviolet Irradiation) influence.Melanin, which has, blocks solar ultraviolet, protects the skin organ below corium, removes and produced in skin histology Raw free free radical, protect the effect of the protein and gene in skin.But because melanin is a kind of thing of stabilization Matter, do not allow to be readily removable after stress disappear, until could remove from skin as the aging of horn cell comes off yet.Cause This, if the hyperpigmentation for damaging beauty, example will occur because environmental factor generates a large amount of unnecessary melanin Such as:Blackening, freckle and spot.With liking the crowd of outdoor activities to increase, it is excessively heavy by the radiation-induced melanin of UV to prevent The demand also is increasing.In order to meet this demand, such as Vitamin C has been used in the skin preparations for extenal use such as cosmetics Acid, kojic acid, ursin etc. have the material of tyrosinase inhibitory activity.But because whitening effect is undesirable and other asks Topic (for example, above-mentioned whitening active thing is added to skin irritatin problem caused in cosmetics, formulation stability problems etc.), So that the use of these compositions is restricted.Tyrosinase inhibitor from plant extracts is lived as potential whitening Property thing, while there is security and the expection to skin low irritant again, at present report (the patent document of existing various exploitations CN201310411195:The detection method of whitening efficacy of melothria heterophylla root extracts;CN201310382406.6:Suspension culture of Aquilaria sinensis pericarp extract Application in skin-lightening cosmetic is prepared).
The reason for skin aging, can be divided into aging caused by light aging and internal cause, and light aging caused by UV exposures can cause The activity increase of dermal elastin enzyme.Elastoser (Elastase) is distributed in Various Tissues and cell, elastin laminin Enzymatic activity increase can cause the hydrolysis of elastic fibers of skin, so as to accelerate the decomposition of intradermal collagen and elastin laminin, make Skin follows the string, and the skin ageing phenomenons such as wrinkle occurs.The anti-aging active thing for being currently known plant origin is flexible Albumen enzyme inhibition, such as indigo plant (patent document CN200680023570.6:Skin preparations for extenal use), sweet pea (patent document CN200680009020.9:Cosmetic preparation containing sweet pea extract) etc..
Yacon (Smallanthus sonchifolius (Poepp.&Endl.) H.Robinson) belongs to composite family sunflower Platymiscium, South America andes region is originated in, introducing the ground such as Yunnan Province of China by Japan at the beginning of 21 century largely cultivates.Yacon original name Ya Gong (yacon), Ya Gong, chrysanthemum potato, saussurea involucrata potato are called, are the traditional food of South America American Indian, have alleviation diabetes etc. more The South America medical and edible dual purpose plant of kind effect.
Yacon root tuber contains substantial amounts of FOS, there is the appellation of " king of FOS ".Also contain in yacon root tuber There are a variety of phenolic acid, terpene and flavone compound.Currently reported yacon leaves extract has anti-oxidant, removing free radical The effect of.
The content of the invention
The invention provides a kind of extracting method of yacon plant extracts, the extracting method is simple to operate, suitable for work Industry metaplasia is produced, and the extract for extracting to obtain by this method has good skin care and whitening effect.
Present invention also offers a kind of yacon plant extracts for extracting to obtain by the above method, the extract has good Good skin care and whitening effect.
Present invention also offers a kind of application process of above-mentioned yacon plant extracts, it can be used as whitening and anti-aging skin The active component of skin external preparation.
A kind of extracting method of yacon plant extracts, including:
(1) in the leaf to pretreated yacon or root tuber, ethanol or ethanol water are added as extractant, Ultrasound, filtering, filtrate concentration;
(2) concentrate for obtaining step (1) carries out further separating-purifying by macroreticular resin, preferably using macropore Resin column chromatography simultaneously uses gradient elution, is first eluted with deionized water, then successively respectively with mass percent concentration by Gradually increased ethanol water carries out gradient elution, and post processing obtains extract.
In step (1), to improve extraction effect, described pretreatment mainly includes the steps such as cleaning, crushing.As excellent Choosing, extractant use ethanol water, and the mass percent concentration of the ethanol water is 50-90%, more preferably 60-80%, it is still more preferably 70%.To ensure that active component as much as possible is extracted.
In step (1), the amount of the extractant once added be generally yacon leaf or 5-15 times of root tuber volume.It is super The sonication time can determine that generally 0.5-2 hours, further is 1-2 hours according to being actually needed.Extraction time is general It can be determined according to being actually needed, preferably, extraction is arrived three times twice, extraction every time is all ultrasonically treated.Extracting temperature can Selection is carried out at room temperature, also can suitably be heated up.
In step (2), during macroporous resin column chromatography, preferably, described macroreticular resin is AB-8 macroporous absorptions Resin.AB-8 macroporous absorbent resins are eluted with deionized water first, mainly remove some water-solubility impurities.Step (2) In, preferably, it is 20-40% ethanol water, matter that the eluant, eluent of the gradient elution, which is followed successively by mass percent concentration, Measure percent concentration be 60-80% ethanol water, mass percent concentration be 90-100% ethanol water, the same to time-division Ethanol eluate is not collected, and three kinds of extracts are prepared after concentration respectively.As further preferred, described eluant, eluent successively Ethanol water that ethanol water that respectively mass percent concentration is 30%, mass percent concentration are 70%, quality Percent concentration is 95% ethanol water.Using the eluant, eluent of concentration stepped change, it is ensured that various in extract solution to have Effect composition is separated, and the active component activity separated is different, during practical application, according to active different, to three kinds The amount of composition is adjusted and selected, to meet the needs of different occasions.
Present invention also offers a kind of yacon plant extracts for extracting to obtain by the above method.The yacon plant carries Thing is taken to be used in different occasions according to being actually needed.
Present invention also offers application process of several above-mentioned yacon plant extracts as skin preparations for extenal use.
The skin preparations for extenal use that a kind of yacon plant extracts acts in preparation with anti-oxidant, radicals scavenging is answered With wherein the yacon plant extracts is prepared by above-mentioned various methods.
When the above-mentioned occasion of application, preferably, when the yacon plant extracts is the Ye Weiyuan using yacon The eluted products for the ethanol water that mass percent concentration is 20-100% are collected during material, during gradient elution.When the saussurea involucrata Fruit plant extracts is when using the root tuber of yacon as raw material, and it is 20-80% to collect mass percent concentration during gradient elution Ethanol water eluted products.As still more preferably, the yacon plant extracts use the leaf of yacon for Raw material, the eluted products for the ethanol water that mass percent concentration is 70-95% are collected during gradient elution.
A kind of yacon plant extracts is preparing the application of the skin preparations for extenal use with anti-aging effect, wherein the snow Lotus fruit plant extracts is prepared by above-mentioned various methods.
When the above-mentioned occasion of application, preferably, collecting the ethanol that mass percent concentration is 60-80% during gradient elution The eluted products of the aqueous solution.As further preferred, the root tuber of yacon is used as raw material.As still more preferably, gradient The eluted products for the ethanol water that mass percent concentration is 70% are collected during elution;The root tuber of yacon is used simultaneously as original Material.
A kind of yacon plant extracts is preparing the application of the skin preparations for extenal use with whitening function, wherein the saussurea involucrata Fruit plant extracts is prepared by above-mentioned various methods.
When the above-mentioned occasion of application, preferably, collecting the second that mass percent concentration is 60-100% during gradient elution The eluted products of alcohol solution.As further preferred, the leaf of yacon is used as raw material, collects quality percentage during gradient elution Specific concentration is the eluted products of 70-95% ethanol water.Still more preferably it is, using the root tuber or Ye Weiyuan of yacon Material, the eluted products for the ethanol water that mass percent concentration is 70% are collected during gradient elution.
As to the preferred of above-mentioned several schemes, described skin preparations for extenal use is cosmetics, particularly Essence cosmetics, The percentage by weight that Smallanthus sonchifolius fruit extract accounts in Essence is 1-10%, more preferably 1-7%.
Composite family Helianthus plant, preferably yacon (Smallanthus are used in the present invention sonchifolius(Poepp.&Endl.)H.Robinson)。
Compared with prior art, beneficial effects of the present invention are embodied in:
The present invention uses leaf or the root tuber of yacon as raw material, by simple extraction process, you can obtain different work Property the extract component with whitening function and anti-aging effect, can be according to being actually needed carry out categorised collection, and enter one Step is prepared into required product, practical, has wide market prospects.
Embodiment
Embodiment 1:The preparation of Smallanthus sonchifolius fruit extract
The yacon leaves or root tuber produced in the present embodiment using Yunnan, but not limited to this.In addition, carried in embodiment The percentage composition arrived, in the case of no specified otherwise, equal representation quality percent concentration.
(1) 70% ethanol 1000mL is added in the leaf of 100g yacons, extraction 2 time ultrasonic 1 hour in room temperature, then Filtering.The solvent under reduced pressure of filtrate is concentrated into 50ml, upper AB-8 resin columns, successively with deionized water, 30% ethanol, 70% ethanol With 95% ethanol elution (each 500ml), it is evaporated under reduced pressure after collecting respectively and removes solvent, obtained drying solid, weigh, obtain saussurea involucrata 30% ethanol position 2.95g of fruit leaf, 70% ethanol position 9.89g, 95% ethanol position 2.45g.
(2) 70% ethanol 1000mL is added in the root tuber of 100g yacons, extraction 2 time ultrasonic 1 hour in room temperature, so After filter.The solvent under reduced pressure of filtrate is concentrated into 50ml, upper AB-8 resin columns, successively with deionized water, 30% ethanol, 70% second Alcohol and 95% ethanol elution (each 500ml), it is evaporated under reduced pressure after collecting respectively and removes solvent, obtained drying solid, weigh, avenged 30% ethanol position 3.0g of lotus fruit block root, 70% ethanol position 3.6g, 95% ethanol position 1.0g.
Embodiment 2:The detection of antioxidation activity
Smallanthus sonchifolius fruit extract is prepared according to embodiment 1, its free-radical scavenging activity is determined with DPPH methods.Determination step is: Smallanthus sonchifolius fruit extract is configured to the aqueous solution (mass-volume concentration 0.05mg/mL) with deionized water respectively, pipette 2mL in In 10mL tool plug test tubes, adding people 2mL DPPH (1,1- diphenyl -2- trinitrophenyl-hydrazines) ethanol solution, (molal volume concentration is 2* 10-4Mol/L), fully mix, be stored at room temperature, the absorbance T of spectrophotometric determination 517nm wavelength is used after 30min;Survey simultaneously Determine 2mL DPPH solution and the mixed absorbance C of 2mL ethanol, 2mL deionized waters and the mixed absorbance C of 2L ethanol0, with And 2mL extract solutions and the mixed absorbance T of 2mL ethanol solutions0.Parallel determination three times, is averaged, according to below equation meter Calculate free radical scavenging activity.
Free radical scavenging activity=[1- (T-T0)/(C-C0)] × 100%.
The measurement result of table 1DPPH method free radical scavenging activities
As shown in Table 1, in the Smallanthus sonchifolius fruit extract used in the present invention, any solvent extractable matter be respectively provided with it is excellent from It is useful as age resister by base scavenging action.During especially with yacon leaves as extraction material, eluant, eluent uses During 70%-95% ethanol water, its free radical scavenging activity is best.Therefore, Smallanthus sonchifolius fruit extract can be coordinated in external application In agent, used as the anti-aging active thing of skin ageing, the skin state of maintenance young healthy is prevented.
Embodiment 3:The detection of elastin laminin enzyme level
The Smallanthus sonchifolius fruit extract prepared respectively according to embodiment 1, is dissolved in deionized water, is configured to the aqueous solution (quality volume Concentration is 0.5mg/ml), for determining elastase inhibitory activity.Determination step is:10 μ L samples are added in 96 orifice plates Solution and 130 μ L contain 1.015mM reaction substrates N- succinyls-propionyl ammonia-propionyl ammonia-propionyl ammonia-paranitroanilinum (English name Succ-Ala-Ala-Ala-pNA, No. CAS:0.1M Tris-Cl cushioning liquid (pH8.0) 52299-14-6), at 25 DEG C Incubate 5 minutes, add 15 μ L elastin laminins enzyme solutions (0.5U/ml), continue to incubate 30min at 25 DEG C, then use ELIASA Determine the absorbance A of 410nm wavelength410.Sample aqueous solution is replaced with deionized water, absorbance is equally determined as reference solution, It the results are shown in Table 2.
Elastase activity inhibiting rate calculation formula is:Inhibiting rate (%)=(1- (A410-C0)/A0) × 100%, wherein A0It is the absorbance of reference solution, A410It is the absorbance of sample solution, C0It is the absorbance of sample solution background.
The measurement result of the elastin laminin enzyme level of table 2
As shown in Table 2, in the Smallanthus sonchifolius fruit extract used in the present invention, the ethanol position of yacon root tuber 70% and saussurea involucrata The ethanol position of fruit leaf 70%, it is respectively provided with and suppresses elastin laminin enzyme effect, yacon root tuber and yacon leaves extract can be matched somebody with somebody Close in external preparation, as preventing skin ageing, maintain the age resister of skin shape of young healthy to use.
Embodiment 4:The detection that tyrosinase activity suppresses
The Smallanthus sonchifolius fruit extract prepared respectively according to embodiment 1, is dissolved in deionized water, is configured to the aqueous solution (quality volume Concentration is 0.5mg/ml), for determining tyrosinase inhibitory activity, using ursin as object of reference.Determination step is:Phosphate delays Rush μ L of solution (pH6.8,30mmol/L) 70, μ L of 1.66mmol/L tyrosine solutions 80, the μ L of sample solution 80 to be well mixed, 37 Incubated 5 minutes in DEG C Water Tank with Temp.-controlled, tyrosinase solution (1000U/ml) 10 μ L are added, after 37 DEG C of constant temperature 10min, with enzyme mark Instrument determines the absorbance A of 475nm wavelength475.Sample aqueous solution is replaced with deionized water, extinction is equally determined as reference solution Degree, the results are shown in Table 3.
Inhibitory activity against tyrosinase calculation formula is:Inhibiting rate (%)=(1- (A475-C0)/A0) × 100%, wherein A0 It is the absorbance of reference solution, A475It is the absorbance of sample solution, C0It is the absorbance of sample solution background.
The measurement result of the tyrosinase inhibitory activity of table 3
As shown in Table 3, each Smallanthus sonchifolius fruit extract used in the present invention all has tyrosinase activity inhibitory action.Its In, the ethanol position of yacon root tuber 70% and the ethanol position of yacon leaves 70% suppression tyrosinase effect are stronger and all excellent In the positive reference substance ursin of same concentrations, yacon root tuber and yacon leaves extract can be coordinated in external preparation, Used as the pigmented whitening active thing of skin is prevented.
Embodiment 5:Skin preparations for extenal use containing Smallanthus sonchifolius fruit extract
70% ethanol 1000mL is added in the root tuber of 100g yacons, in room temperature ultrasound 1 hour, is extracted 2 times, then mistake Filter.The solvent under reduced pressure of filtrate is concentrated into 50ml, upper AB-8 resin columns, successively with deionized water, 30% ethanol, 70% ethanol and 95% ethanol elution (each 500ml), removing solvent is evaporated under reduced pressure after collecting 70% alcohol elution, obtains yacon root tuber 70% ethanol position, the preparation for skin preparations for extenal use.Percentage by weight of the Smallanthus sonchifolius fruit extract in skin preparations for extenal use It is 1-10%, preferably 1-7%.It is the embodiment of concrete application of the yacon root tuber in skin preparations for extenal use below.In table 4 below "-" represents no added.
Embodiment 6:Essence containing yacon root tuber
Yacon root tuber extract is taken, for preparing the Essence with whitening function, the component that the Essence contains As shown in table 4:
Table 4
Above is invention preferred embodiment, is not intended to limit the invention.

Claims (8)

1. a kind of extracting method of yacon plant extracts, including:
(1) in the leaf to pretreated yacon or root tuber, add ethanol or ethanol water is used as extractant, it is super Sound, filtering, filtrate concentration;
(2) concentrate for obtaining step (1) carries out the further separating-purifying of column chromatography by macroreticular resin, and uses gradient Elution, is first eluted, then with mass percent concentration, gradually increased ethanol water enters respectively successively with deionized water Row gradient elution, post processing obtain extract;
Described macroreticular resin is AB-8 macroporous absorbent resins;
It is 20-40% ethanol water, mass percent that the eluant, eluent of the gradient elution, which is followed successively by mass percent concentration, The ethanol water that ethanol water that concentration is 60-80%, mass percent concentration are 90-100%.
2. a kind of yacon plant extracts, it is characterised in that the yacon plant extracts is as the side described in claim 1 Method is extracted to obtain.
3. a kind of yacon plant extracts is preparing the application of skin preparations for extenal use, it is characterised in that the yacon plant carries Thing is taken to be prepared as the method described in claim 1.
4. yacon plant extracts according to claim 3 is preparing the application of skin preparations for extenal use, it is characterised in that institute The skin preparations for extenal use stated is cosmetics.
5. yacon plant extracts according to claim 4 is preparing the application of skin preparations for extenal use, it is characterised in that institute The skin preparations for extenal use stated is Essence cosmetics, and the percentage by weight that Smallanthus sonchifolius fruit extract accounts in Essence is 1-10%.
6. yacon plant extracts according to claim 3 is preparing the application of skin preparations for extenal use, it is characterised in that when The yacon plant extracts is when using the leaf of yacon as raw material, and collecting mass percent concentration during gradient elution is The eluted products of 20-100% ethanol water;When the yacon plant extracts be use yacon root tuber for raw material When, the eluted products of the ethanol water that mass percent concentration is 20-80% are collected during gradient elution.
7. yacon plant extracts according to claim 3 is preparing the application of skin preparations for extenal use, it is characterised in that adopts It is raw material with the root tuber of yacon;The elution for the ethanol water that mass percent concentration is 60-80% is collected during gradient elution Product.
8. yacon plant extracts according to claim 3 is preparing the application of skin preparations for extenal use, it is characterised in that adopts It is raw material with the root tuber or leaf of yacon, the ethanol water that mass percent concentration is 70-95% is collected during gradient elution Eluted products.
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