CN101336874A - Water-solubility active extract in fruit skin, preparation method and use thereof - Google Patents
Water-solubility active extract in fruit skin, preparation method and use thereof Download PDFInfo
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- CN101336874A CN101336874A CNA2008100219013A CN200810021901A CN101336874A CN 101336874 A CN101336874 A CN 101336874A CN A2008100219013 A CNA2008100219013 A CN A2008100219013A CN 200810021901 A CN200810021901 A CN 200810021901A CN 101336874 A CN101336874 A CN 101336874A
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Abstract
The invention relates to a water-soluble active extract derived from fruit peels, the preparation method and the application thereof. The fruit peel is treated by the steps of drying, pulverization, extraction, flocculation, separation and concentration, to prepare a water-soluble active extract. Then, the extract is added in cosmetic matrixes to allow a cosmetic to have skin-whitening and anti-skin ageing functions. The fruit peel extract is obtained after the screening of tyrosinase-inhibiting, antioxidant and free radical-scavenging activities in the water-soluble extracts of fruit peels such as Citrus peels, and has skin-whitening and anti-skin ageing effects. The water-soluble active extract has the advantages of easily-accessible raw materials, renewable resources and simple preparation method. The obtained extract has good stability and durable effect and serves as cosmetic additives in any stage of cosmetic production, without the risks of solvent residue and microbial contamination.
Description
Technical field
The present invention relates to the functional cosmetics of peel extract and Pear Power and activity of fighting against senium, specifically, relate to a kind of water-soluble active thing that from peel, extracts and (contain a large amount of natural fruit flavone and fruit polyphenol, wherein comprise flavonoid glycoside flavone and polymethoxyflavone flavonoid etc.), and use this extract and prepare Pear Power and anti-aging cosmetics.
Background technology
Skin is human maximum organ, and its structure elaborate is human natural protection barrier.But along with the increase at age and the erosion of environment, its defense function can be destroyed.External pressure such as ultraviolet radiation, and the emotion of intrinsic pressure such as anxiety all can produce a large amount of free radicals, and it encroaches on skin histology, make skin become coarse, produce black speck, wrinkle etc., quicken the aging of skin.
Contain nutrients such as abundant vitamin C and saccharide in the fruit, these nutrient substance have excellent physiologically active but are extremely unstable.In the evolutionary process of plant, fresh fruit need be stored nutrient substance and guarantee that it is not damaged, so formed its perfect preventing mechanism.Discover, often contain a large amount of antibiotic substance, antioxidant in the peel, and store moisture and nutriment by forming fine and close structure.For example, Pericarpium Citri Reticulatae has had the history in thousands of years as the Chinese crude drug medication, contains unusual abundant tangeritin in the Pericarpium Citri Reticulatae, comprises flavonoid glycoside such as Pericarpium Citri Reticulatae glycosides and neohesperidin etc., and polymethoxyflavone class such as Nobiletin etc.These tangeritins have different physiological roles, as (1) antioxidation, free radical resisting, and (2) antiinflammatory, antiallergic, (3) are anticancer, (4) prevention cardiovascular and cerebrovascular disease etc.Contain abundant apple polyphenol and flavonoid class material in the Pericarpium Mali pumilae, have excellent antioxidation and anti-radical action.
CN100389798C discloses a kind of Fructus Litchi extract and its production and use, and it adopts supercritical process to extract, and extract obtainedly can be used for preparing cancer therapy drug and food additive and cosmetics; CN1961858A then discloses a kind of rue family citrus plant pericarp extract and its production and use, adopt ethanol extraction, filtrate is passed through absorption with macroporous adsorbent resin, eluent is through defat, drying and pulverizing, extract, this extract will be used to prepare the cosmetics that have anti-sunlight function in UVA district and UVB district.There are all deficiencies in said method, and its range of application also is restricted.Therefore, people are very limited to the research and the utilization of plant peel, and the abundant fruit resource of nature still eats and rolls juice with fresh fruit at present and is processed as the master, and a large amount of peels is thrown away in vain as waste material.
Summary of the invention
The present invention is intended to use for reference the natural protection mechanism of plant, extracts the natural stable water-soluble active ingredient with defying age and white-skinned face function from depleted plant peel, and be applied to whiten and antidotal cosmetics in.
Technical solution of the present invention is:
Water-soluble active preparation method of extract in the peel may further comprise the steps:
Step 1, exsiccant fruit peel powder is broken into powder;
Step 2, the amount of pressing the weight ratio 1: 2～10 of peel powder and distilled water add in the extractor, heat and boil, and precipitation is removed in cooling back centrifugalize, gets the crude extract that supernatant obtains peel;
Step 3, the crude extract of peel is added volume ratio is 1: 1～10 ethanol, perhaps adds chitin according to ethanol volume and peel mass ratio 10～100: 1, leaves standstill after the stirring, treat that pectin flocculates fully after, pass through the centrifugalize disgorging, get supernatant;
Step 4, the supernatant that step 3 is obtained filter, and concentrated filtrate obtains the peel water solubility extract, regulates about its PH to 5.0～7.0, is dried into extractum under 40～48 ℃ of conditions.
Further, water-soluble active preparation method of extract in the above-mentioned peel, wherein---
In the step 1, the fresh peel of cleaning is descended dry 48 hours at 45 ℃, and then be ground into the powder of particle mean size about 100 orders;
In the step 2, add extractor by the consumption of 1 kilogram of peel powder and 10 liters of distilled water, heat and boiled 30 minutes, cooling is removed precipitation afterwards with 4500rpm rotating speed centrifugalize 30 minutes, gets the crude extract that supernatant obtains peel;
In the step 3, be to add ethanol at 1: 1.5 by volume, stir and left standstill 2 hours after 2 minutes the peel crude extract that obtains, treat that pectin flocculates fully after, with 4500rpm rotating speed centrifugalize 30 minutes, disgorging;
In the step 4, filtrate concentrates by distilling under reduced pressure, controls distillatory temperature about 45 ℃, the recycling of resulting alcohol solvent fraction.
Further, in the above-mentioned preparation method, described peel is one or more in the following group---peel of Citrus reticulata Blanco, Pericarpium Mali pumilae, Pericarpium Pyri, Exocarpium Citrulli, Pericarpium Granati, litchi rind, Pericarpium Vitis viniferae, grape skin, Garcinia mangostana skin, Ribes nigrum L. skin, Fructus Pruni skin, peach skin, Lee's skin, peel of Fructus Pruni pseudocerasi.
Water-soluble active extract in a kind of peel is prepared from by above-mentioned preparation method.This extract can be used for preparing the functional cosmetic with restraint of tyrosinase activity and non-oxidizability.
A kind of whitening and anti-aging active cosmetic includes water-soluble active extract in the aforementioned peel, and the dosage form of cosmetics is not limit, and can be water preparation, cream, oil preparation, washing liquid or emulsion etc.
Compared with prior art, the present invention has following advantage:
1, in the selection of the functional raw material of cosmetics, the peel source is abundant, with low cost, production be again high value added product, really realized turning waste into wealth, have very high economic benefit;
2, in the extraction scheme of above-mentioned peel, used raw material does not have the raw material that limits the use of of cosmetics, therefore can be added directly in the cosmetics, need not to scruple the residual solvent problem, and existing many peels and extraction process is used methanol, acetone and other organic solvent must thoroughly be removed these organic solvents before use, makes trouble to production technology;
3, adopt ethanol precipitation pectin in said extracted technology, compare other intermediate processing, Ethanol Method pectin precipitation is more complete, and antioxidant activity and the active ingredient loss of whitening are less, and ethanol also can recycling, saves cost;
4, process high-temperature boiling in above-mentioned preparation technology, the activated feedstock that is extracted has good high-temperature stability, can be added on arbitrary stage of cosmetic formulations, even add in high temperature sterilize stage of cosmetics and also can not influence its original activity, thereby need not to scruple the cold microbiological pollution that may bring of joining of cosmetics.
The specific embodiment
The present invention is applied to the protection mechanism of occurring in nature peel in the skin nursing; prepare the cosmetics of Pear Power anti-aging effects; it is primary raw material that these cosmetics are selected the plant peel for use, therefrom extracts natural water-soluble active thing, the function that has free radical resisting, antioxidation and whiten.
The present invention extracts the water-soluble active thing from peel method may further comprise the steps:
Step 1, exsiccant fruit peel powder is broken into powder;
Step 2, the amount of pressing the weight ratio 1: 2～10 of peel powder and distilled water add in the extractor, heat and boil 30 minutes, and cooling back 4500rpm removed precipitation in centrifugal 20～40 minutes, got the crude extract that supernatant obtains peel;
Step 3, the crude extract of peel is added volume ratio is 1: 1～10 ethanol, perhaps add chitin according to ethanol volume and peel weight ratio 10～100: 1, stir and left standstill 1～4 hour after 1～5 minute, after treating that pectin flocculates fully, through centrifugal 20～40 minutes disgorging of 4500rpm, get supernatant;
Step 4, the supernatant that step 3 is obtained filter, and concentrated filtrate obtains the peel water solubility extract, also about its PH to 5.0 of scalable～7.0, is dried into extractum at 45 ℃ at last.
The selection process of such scheme is:
In the step 1 of such scheme, the fresh peel that employing will be cleaned is ground into the powder of particle mean size about 100 orders 45 ℃ of down dry 48 hours (cold preservation are standby).Described fruit peel includes but not limited to: peel of Citrus reticulata Blanco, Pericarpium Mali pumilae, Pericarpium Pyri, Exocarpium Citrulli, Pericarpium Granati, litchi rind, Pericarpium Vitis viniferae, grape skin, Garcinia mangostana skin, Ribes nigrum L. skin, and drupe class peel such as Fructus Pruni, peach, Lee, Fructus Pruni pseudocerasi.
In the step 2 of such scheme, add extractor by the consumption of 1 kilogram of peel powder and 10 liters of distilled water, to heat and boiled 30 minutes, cooling afterwards 4500rpm was removed precipitation in centrifugal 30 minutes, got the crude extract that supernatant obtains peel.
In the step 3 of such scheme, be to add ethanol at 1: 1.5 by volume with the peel crude extract that obtains, stir after 2 minutes, left standstill 2 hours, treat that pectin flocculates fully after, centrifugal 30 minutes disgorging of 4500rpm.
In the step 4 of such scheme, concentrate by distilling under reduced pressure concentrating the peel aqueous solution that obtains, control distillatory temperature about 45 ℃, resulting alcohol solvent fraction can recycling.
The active matter that adopts such scheme to obtain has good high-temperature stability, the inventor is to intermediate product of producing and the extractum of finally making, carry out the active detection of antioxidation, free radical resisting and restraint of tyrosinase, discovery active component in preparation process obtains good enrichment and reservation, and the water solubility extract of acquisition has higher activity.Its effect detection method is as follows:
One, the active detection method of restraint of tyrosinase
1, gets four test tubes and put on 1 respectively
#, 2
#, 3
#, 4
#
2,, in vitro add the corresponding listed reactant liquor that respectively is listed as respectively at four with reference to table 1;
3, jolting mixing, 37 ℃ of preheating 10min;
4, add tryrosinase solution respectively at each pipe then, 37 ℃ of accurate response 20min are transferred to rapidly in the cuvette, survey absorbance (A) in the 475nm place;
5, the calculating of tyrosinase inhibition rate: be calculated as follows to tyrosinase inhibition rate.
Suppression ratio=[1-(A3-A4)/(A1-A2)] * 100%
In the formula: A1, A2, A3, A4 represent in the table 11 respectively
#, 2
#, 3
#, 4
#Four reaction systems measured absorbance A in step 4
475
Table 1: the composition (unit: ml) of liquid to be measured
| Reactant liquor | 1 # | 2 # | 3 # | 4 # |
| Tyrosine solution | 0.7 | 0 | 0.7 | 0 |
| Whitening agent solution | 0 | 0 | 0.5 | 0.5 |
| The blank solvent of whitening agent | 0.5 | 0.5 | 0 | 0 |
| The PH6.8 phosphate buffer | 0.8 | 1.5 | 0.8 | 1.5 |
Two, the external detection method of active matter free radical resisting ability
1, accurately take by weighing 20mg DPPH (1,1-dimethyl benzyl phenylhydrazine, C
18H
12N
5O
6), use the dehydrated alcohol standardize solution in the 250ml volumetric flask, concentration 2 * 10
-4Mol/L;
2, get some test tube numberings,, add reagent with reference to table 2.
Table 2: reagent addition (unit: ml)
| Group | DPPH | Sample | Extract solvent |
| Blank 0 | 2.0 | 0 | 1.0 |
| Sample solution 1 | 2.0 | 1.0 | 0 |
| Sample solution 2 | 2.0 | 1.0 | 0 |
| Sample solution 3 | 2.0 | 1.0 | 0 |
3, mix homogeneously behind (25 ℃ or water-bath 25 ℃) reaction 10min, is measured the absorbance under the 517nm wavelength under the room temperature.
4, calculate suppression ratio according to following formula:
Suppression ratio (%)=(1-A
t/ A
Blank) * 100%
A
Blank: the absorbance of blank under the 517nm wavelength
A
t: the absorbance of sample under the 517nm wavelength
Three, the external detection method of active matter Total antioxidant capacity
(1) solution preparation
1, FRAP working solution
The A-acetate buffer solution: get sodium acetate 5.1g, add glacial acetic acid 20ml, thin up promptly gets " acetic acid-sodium acetate " buffer of PH3.6 to 250ml again
B-TPTZ solution: 10mmol/L TPTZ+40mmol/L HCl (final concentration)
The FeCl of C-liquor ferri trichloridi: 20mmol/L
36H
2O
D-FRAP working solution: 25ml A+2.5ml B+2.5ml C
2, sample solution
A: take by weighing sample, be made into the solution of 10g/100ml with acetate buffer solution;
B: with the Vc solution of acetate buffer solution preparation 2mmol/L.
(2) operational approach
1, the making of standard curve:
1) gets freshly prepared FRAP 200 μ l (water-bath is preheating to 37 degree) and add 40 μ l deionized waters, under the 593nm wavelength, do the dummy absorbance correction with spectrophotometer;
2) with reference to table 3 preparation Vc standard solution;
3) respectively 10 μ l standard solution and 30 μ l deionized waters are added in the FRAP working solution of 200 μ l mix homogeneously;
4) write down light absorption value after 0.5 second by spectrophotometer;
5) according to the content production standard curve of absorbance and Vc.
The configuration of table 3:Vc standard solution
| Ultimate density (mmol/L) | 0.1 | 0.2 | 0.4 | 0.6 | 0.8 | 1.0 | 1.2 | 1.4 | 1.6 | 1.8 | 2.0 |
| 2mmol/L Vc solution (μ l) | 5 | 10 | 20 | 30 | 40 | 50 | 60 | 70 | 80 | 90 | 100 |
| Deionized water (μ l) | 95 | 90 | 80 | 70 | 60 | 50 | 40 | 30 | 20 | 10 | 0 |
2, the mensuration of sample oxidation resistance
Utilize the method in 1 to measure its absorbance value the sample solution that configures, on standard curve, find its corresponding V content, relatively the sample of equal quality and the antioxidant effect of Vc.
By above active the detection, find: the activity of the active matter restraint of tyrosinase that the present invention extracts and the Vc of equal quality are approaching, its non-oxidizability and free radical resisting effect are also approaching with Vc, but the active matter that the method is extracted has good heat stability and light stability.
According to the peel extract that technical solution of the present invention makes, can be used as the functional raw material of whitening with anti-aging cosmetics, its type of service does not have specific (special) requirements, and the form that it can be formulated into has water preparation, cream, oil preparation, washing liquid, emulsion etc.
Typical substrate as the present invention's application, the known substance that relates to has: vegetable and animals oils, mineral oil, wax, higher alcohol, aliphatic alcohol, silicone oil, surfactant, phospholipid, alcohols, polyalcohols, water-soluble polymer, oil-soluble polymers class, mineral, deionized water etc., in addition, can suitably add PH regulator, antioxidant, chelating agen, pigment, antiseptic and essence etc. as required.In addition, also can be used in combination, as sunscreen, blood circulation accelerant, disinfectant, antiinflammatory, cell activator, vitamins, amino acids, wetting agent, keratolytic agent with other active component of Pear Power effect, anti-aging effects or skin-care effect effect.
Table 4 and table 5 are respectively to use the peel extract preparation " cream frost " of the present invention's acquisition and the concrete batching composition of " moisturizer " cosmetics.During preparation, component A is heated to 85 ℃ in will showing, and dissolves to stir, as oil phase, B component to be put into container be heated to 85 ℃, stirring and dissolving becomes the water raw material, stir in the oil phase raw material adding water raw material, behind the emulsifying homogenizing, add component C when being cooled to 65 ℃, continue to stir when being cooled to 35 ℃, add peel extract and essence, antiseptic, stir, ageing gets final product fill after 24 hours, bag changes, checks, and makes the present invention's example product.
Table 4: " cream frost " batching
Table 5: " moisturizer " batching
Adopt " double-blind method " test evaluation whitening effect of the present invention: contain the whitening anti-aging product of peel extract and do not contain each portion of substrate of peel extract according to above-mentioned examples preparation, the former is as sample, the latter is product in contrast, and the Ms who selects 25～60 years old is as the experiment group member.Sooner or later face and each four position of forearm every group member after washing one's face every day are coated with an amount of preparation, totally 4 weeks, use the content of skinanalysis apparatus test dermal melanin, and the skin color difference meter is assessed the whitening effect of preparation, utilize the skin elasticity tester to test skin elasticity simultaneously, and skin microscope and the viable skin surface analysis system depth of testing the wrinkle of skin, thereby estimate the defying age effect of preparation.The result shows (correction data preferably is provided): contain the cosmetics of peel extract, have significantly whiten and anti-water active always.
Claims (10)
1, water-soluble active preparation method of extract in the peel may further comprise the steps:
Step 1, exsiccant fruit peel powder is broken into powder;
Step 2, the amount of pressing the weight ratio 1: 2～10 of peel powder and distilled water add in the extractor, heat and boil, and precipitation is removed in cooling back centrifugalize, gets the crude extract that supernatant obtains peel;
Step 3, the crude extract of peel is added volume ratio is 1: 1～10 ethanol, perhaps adds chitin according to ethanol volume and peel mass ratio 10～100: 1, leaves standstill after the stirring, treat that pectin flocculates fully after, pass through the centrifugalize disgorging, get supernatant;
Step 4, the supernatant that step 3 is obtained filter, and concentrated filtrate obtains the peel water solubility extract, regulates about its PH to 5.0～7.0, is dried into extractum under 40～48 ℃ of conditions.
2, water-soluble active preparation method of extract in the peel according to claim 1 is characterized in that: in the step 1, the fresh peel of cleaning is descended dry 48 hours at 45 ℃, and then be ground into the powder of particle mean size about 100 orders.
3, water-soluble active preparation method of extract in the peel according to claim 1, it is characterized in that: in the step 2, consumption by 1 kilogram of peel powder and 10 liters of distilled water adds extractor, heating was also boiled 30 minutes, the cooling back was with 4500rpm rotating speed centrifugalize 30 minutes, remove precipitation, get the crude extract that supernatant obtains peel.
4, water-soluble active preparation method of extract in the peel according to claim 1, it is characterized in that: in the step 3, with the peel crude extract that obtains is 1: 1.5 adding ethanol by volume, stir and left standstill 2 hours after 2 minutes, after treating that pectin flocculates fully, with 4500rpm rotating speed centrifugalize 30 minutes, disgorging.
5, water-soluble active preparation method of extract in the peel according to claim 1, it is characterized in that: in the step 4, filtrate concentrates by distilling under reduced pressure, controls distillatory temperature about 45 ℃, the recycling of resulting alcohol solvent fraction.
6, water-soluble active preparation method of extract in the peel according to claim 1 is characterized in that: described peel is one or more in the following group---peel of Citrus reticulata Blanco, Pericarpium Mali pumilae, Pericarpium Pyri, Exocarpium Citrulli, Pericarpium Granati, litchi rind, Pericarpium Vitis viniferae, grape skin, Garcinia mangostana skin, Ribes nigrum L. skin, Fructus Pruni skin, peach skin, Lee's skin, peel of Fructus Pruni pseudocerasi.
7, water-soluble active extract in a kind of peel is prepared from by any one preparation method of claim 1～6.
8, the water-soluble active extract has purposes in the functional cosmetics of restraint of tyrosinase activity and non-oxidizability in preparation in the described peel of claim 7.
9, a kind of whitening and anti-aging active cosmetic is characterized in that: comprise water-soluble active extract in the described peel of claim 7.
10, according to claim 9 whitening and anti-aging active cosmetic is characterized in that: these cosmetics are water preparation, cream, oil preparation, washing liquid or emulsion.
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