CN103948670A - Preparation method and applications of mung bean peel effective component - Google Patents
Preparation method and applications of mung bean peel effective component Download PDFInfo
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Abstract
The invention relates to a preparation method and applications of a mung bean peel effective component, and belongs to the field of traditional Chinese medicine effective component extraction. The preparation method comprises following steps: a, mung bean peel is collected, is extracted with water, is subjected to filtration and condensation, is diluted with water, and is filtered so as to obtain a sample liquid; b, the sample liquid is subjected to HPD450 macroporous resin absorption, is subjected to elution with water to be colorless, and is subjected to elution with ethanol so as to obtain an eluent, and the eluent is filtered and condensed so as to obtain the mung bean peel effective component. Beneficial effects of the preparation method are that: the preparation method is capable of increasing product purity, and reducing production cost; production equipment is simple; efficiency is high; and the preparation method is suitable for large-scale production. The mung bean peel effective component is capable of resisting oxidation, resisting aging, protecting skin, delaying skin aging, and the like; and can be used as additives or raw materials of food, health products, cosmetics, and medicines.
Description
Technical field
The invention belongs to Chinese medicine active component and extract field, be specifically related to a kind of preparation method and purposes of Testa Phaseoli radiati active component.
Background technology
Testa Phaseoli radiati is to rub the seed coat getting off after steep raising Semen phaseoli radiati.Compendium of Material Medica is carried: for relieving heat toxin, move back corneal nebula.Testa Phaseoli radiati is common mung bean products processing, mostly uses as feedstuff, does not obtain sufficient development and utilization.
Cheng Shuan etc. carry in " preliminary study of antioxidant in Testa Phaseoli radiati ": utilize methanol from Testa Phaseoli radiati, to extract Flavonoid substances for antioxidation, the extraction ratio of its flavone compound is 1.32%.
In " Study on extraction of total flavones in Testa Phaseoli radiati " literary composition, carry: utilize Testa Phaseoli radiati, extraction time 150min, volume fraction of ethanol 50%, extracts 80 DEG C of temperature, solid-to-liquid ratio 1:10, extraction time 2 times, in Testa Phaseoli radiati, the extracted amount of total flavones is 3.879mg/g.
Also have in " extraction of flavonoid compounds in mung bean hull and quantitative assay " literary composition and carry: the optimum extraction process of having inquired into flavonoid compounds in mung bean hull with orthogonal experiment.Result of study shows: at 70 DEG C with 6 times to the alcohol reflux of Semen phaseoli radiati tare weight volume 30% 2 times, each 2h, Testa Phaseoli radiati flavone compound extraction effect is best.(the NO of Al for sample
3)
3colorimetry is measured under 510nm, and rutin is criterion calculation content, and the average content that obtains flavonoid compounds in mung bean hull is 1.459%.
Application number is that 201110203090.0 Chinese invention patent " a kind of method of extracting anti-oxidant mung bean polysaccharide " discloses and a kind ofly from Testa Phaseoli radiati, extracts mung bean polysaccharide for antioxidation method.
But the existing composition that utilizes Testa Phaseoli radiati to propose is not remarkable for antioxidative action effect, also exists the inadequate shortcoming of extracts active ingredients, has caused the waste of resource.
Summary of the invention
The object of this invention is to provide a kind of preparation method and purposes of Testa Phaseoli radiati active component.
Testa Phaseoli radiati active component of the present invention, its preparation process comprises the following steps:
A, get Testa Phaseoli radiati, extracting in water, filters, concentrated, and thin up filters, and obtains sample solution;
B, by after HPD450 absorption with macroporous adsorbent resin on described sample solution, first wash with water to colourless, and then with ethanol elution, obtain eluent, filter, concentrated, obtain Testa Phaseoli radiati active component.
As preferably, the number of times extracting in described step a is 1～3 time, and the time of extraction is 1～3 hour.
As preferably, in described step a when extracting in water, the weight adding water is described Testa Phaseoli radiati 8～20 times.Particularly preferred, in described step a when extracting in water, the weight adding water is described Testa Phaseoli radiati 10 times, 12 times, 14 times, 16 times and 18 times.
As preferably, in described step a, concentrate and adopt concentrating under reduced pressure.
As preferably, in described step a, being concentrated into proportion is 1.05～1.075.
As preferably, in described step b, the mass percent concentration of ethanol is 70%～90%.
As preferably, in described step b, being concentrated into proportion is 1.15～1.175.
Further, the present invention also provides the Testa Phaseoli radiati active component that a kind of described preparation method makes.
Further, the present invention also provides a kind of described Testa Phaseoli radiati active component in the application of preparing in anti-oxidation medicine.
Further, the present invention also provides a kind of cosmetic composition with anti-oxidation function that utilizes described Testa Phaseoli radiati active component to make, this cosmetic composition is composed of the following components: by weight, and 1,600～800 parts of 3-butanediols, 50～150 parts of Testa Phaseoli radiati active components, 200～400 parts of purified water, 0.005～0.015 part of phenoxyethanol.Particularly preferred, this cosmetic composition is composed of the following components: by weight, and 1,700 parts of 3-butanediols, 100 parts of Testa Phaseoli radiati active components, 300 parts of purified water, 0.01 part of phenoxyethanol.Wherein, in Testa Phaseoli radiati active component, add 1,3-butanediol, purified water, contribute to said composition compatible with other supplementary material, form stable cosmetics finished product.Add phenoxyethanol for anticorrosion.
In the present invention, can be with above-mentioned cosmetics or directly taking Testa Phaseoli radiati active component as basic ingredient, then be equipped with other supplementary material, make cosmetics finished product according to the common process of preparing cosmetics.
Beneficial effect of the present invention is: taking Testa Phaseoli radiati as raw material, work out a kind of preparation method of preparing Testa Phaseoli radiati active component.The method has improved the purity of product, has reduced production cost, and production equipment is simple, and efficiency is high, is applicable to large-scale production.This active component has antioxidation, defying age, protection skin, delay skin aging isoreactivity, can be for the additive of food, health product, cosmetics and medicine or as raw material.
Brief description of the drawings
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, below the accompanying drawing of required use during embodiment is described is briefly described.
Fig. 1 is Testa Phaseoli radiati active component reducing power test pattern;
Fig. 2 is the test pattern of Testa Phaseoli radiati active component to the effect of DPPH free radical scavenging;
Fig. 3 is the test pattern of the scavenging action of Testa Phaseoli radiati active component to superoxide anion;
Fig. 4 is the test pattern of Testa Phaseoli radiati active component to copper ion sequestering power;
Fig. 5 is Testa Phaseoli radiati active component and the test pattern of Semen phaseoli radiati seed active component to the effect of DPPH free radical scavenging.
Detailed description of the invention
For making those skilled in the art understand in detail production technology of the present invention and technique effect, further introduce application of the present invention and technique effect with concrete production instance below.
Embodiment 1:
A, get Testa Phaseoli radiati, add the water extraction 2 times of 10 times of weight, each time of extracting is 2 hours, employing has 200 object filter screens and filters, being evaporated to proportion is 1.06(heat determination), subsequently taking concentrated solution as fundamental unit, add 4 times of weight water dilutions, adopt filter cloth to filter, obtain sample solution;
B, by after HPD450 absorption with macroporous adsorbent resin on described sample solution, first wash with water to colourless, and then with mass percent concentration be 75% alcoholic solution eluting, flow velocity is 2BV/ hour, obtain eluent, employing has 300 object filter screens filters, and concentrated proportion is 1.15(heat determination), obtain Testa Phaseoli radiati active component.
Embodiment 2:
A, get Testa Phaseoli radiati, add the water extraction 1 time of 20 times of weight, 1 hour extraction time, employing has 200 object filter screens filters, and being evaporated to proportion is 1.07(heat determination), subsequently taking concentrated solution as fundamental unit, add 5 times of weight water dilutions, adopt filter cloth to filter, obtain sample solution;
B, by after HPD450 absorption with macroporous adsorbent resin on described sample solution, first wash with water to colourless, and then with mass percent concentration be 70% alcoholic solution eluting, flow velocity is 2BV/ hour, obtain eluent, employing has 300 object filter screens filters, and concentrated proportion is 1.17(heat determination), obtain Testa Phaseoli radiati active component.
Embodiment 3:
A, get Testa Phaseoli radiati, add the water extraction 3 times of 8 times of weight, each time of extracting is 3 hours, employing has 200 object filter screens and filters, being evaporated to proportion is 1.06(heat determination), subsequently taking concentrated solution as fundamental unit, add 3 times of weight water dilutions, adopt filter cloth to filter, obtain sample solution;
B, by after HPD450 absorption with macroporous adsorbent resin on described sample solution, first wash with water to colourless, and then with mass percent concentration be 90% alcoholic solution eluting, flow velocity is 2BV/ hour, obtain eluent, employing has 300 object filter screens filters, and concentrated proportion is 1.16(heat determination), obtain Testa Phaseoli radiati active component.
Embodiment 4:
A, get Testa Phaseoli radiati, add the water extraction 2 times of 14 times of weight, each time of extracting is 3 hours, employing has 200 object filter screens and filters, being evaporated to proportion is 1.06(heat determination), subsequently taking concentrated solution as fundamental unit, add 3 times of weight water dilutions, adopt filter cloth to filter, obtain sample solution;
B, by after HPD450 absorption with macroporous adsorbent resin on described sample solution, first wash with water to colourless, and then with mass percent concentration be 90% alcoholic solution eluting, flow velocity is 1.5BV/ hour, obtain eluent, employing has 300 object filter screens filters, and concentrated proportion is 1.16(heat determination), obtain Testa Phaseoli radiati active component.
Comparative example 1:
Get 10 times of water gagings of Testa Phaseoli radiati and decoct 2 times, each time decocting is 2 hours, obtains Testa Phaseoli radiati water extract.
Comparative example 2:
To get 10 times of amount mass percent concentrations of Testa Phaseoli radiati be 50% ethanol extraction 2 times extracts 2 hours at every turn, obtains Testa Phaseoli radiati alcohol extract.
Comparative example 3:
To get 10 times of amount mass percent concentrations of Testa Phaseoli radiati be 30% ethanol extraction 2 times extracts 2 hours at every turn, obtains Testa Phaseoli radiati alcohol extract.
For checking effect of the present invention, spy makes following contrast test:
| Product | General flavone content |
| Embodiment 1 | 7.35mg/ml |
| Embodiment 2 | 6.28mg/ml |
| Embodiment 3 | 8.12mg/ml |
| Embodiment 4 | 5.32mg/ml |
| Comparative example 1 | 0.535mg/ml |
| Comparative example 2 | 0.380mg/ml |
| Comparative example 3 | 0.345mg/ml |
As seen from the above table, in Testa Phaseoli radiati active component by preparation method gained of the present invention, general flavone content is higher, separately owing to passing through HPD450 resin concentration total flavones, can effectively avoid the impurity strippings such as chlorophyll in Testa Phaseoli radiati active component, thereby ensure the purity of Testa Phaseoli radiati active component.
Separately the research of DPPH free radical scavenging effect is relatively found with comparative example 1-3 gained active component and extract by embodiment 1-4, in embodiment, the oxidation resistance of the Testa Phaseoli radiati active component of gained is 4-6 times extract obtained in comparative example.
Embodiment 5:
For effectively preserving Testa Phaseoli radiati active component, be applied to better in cosmetics.The Testa Phaseoli radiati active component of embodiment 1-4 gained can be equipped with to other component and make the required compositions of cosmetics.Said composition is composed of the following components: by weight, gets 1,0.01 part of 700 parts of 3-butanediols, 100 parts of Testa Phaseoli radiati active components, 300 parts of purified water and phenoxyethanol, mixes, and packaging.
Embodiment 6:
For effectively preserving Testa Phaseoli radiati active component, be applied to better in cosmetics.The Testa Phaseoli radiati active component of embodiment 1-4 gained can be equipped with to other component and make the required compositions of cosmetics.Said composition is composed of the following components: by weight, gets 1,0.015 part of 600 parts of 3-butanediols, 150 parts of Testa Phaseoli radiati active components, 200 parts of purified water and phenoxyethanol, mixes, and packaging.
Embodiment 7:
For effectively preserving Testa Phaseoli radiati active component, be applied to better in cosmetics.The Testa Phaseoli radiati active component of embodiment 1-4 gained can be equipped with to other component and make the required compositions of cosmetics.Said composition is composed of the following components: by weight, gets 1,0.005 part of 800 parts of 3-butanediols, 50 parts of Testa Phaseoli radiati active components, 400 parts of purified water and phenoxyethanol, mixes, and packaging.
For verifying technique effect of the present invention, test below special work:
1, Testa Phaseoli radiati active component reducing power test
Experimental principle: reducing power is one of index of the potential oxidation resistance of material, and potassium ferricyanide is reduced into potassium ferrocyanide by sample, potassium ferrocyanide and Fe
3+effect generates Prussian blue, measures light absorption value to detect Prussian blue growing amount at 700nm place, weighs the reducing power of sample by Prussian blue growing amount.
Experimental technique: get respectively Testa Phaseoli radiati active component solution 0.1mL to be measured, 0.2mL, 0.5mL, 1mL, volume is supplied to 1mL with distilled water; Get positive control sample vitamin c solution 0.1mL, 0.2mL, 0.5mL, 1mL, supply 1mL with distilled water.In each group of sample, add 1mL phosphate buffer and 1mL potassium ferricyanide solution, mix, 50 DEG C of water-bath 20min, take out, and add 1mL trichloroacetic acid solution, mix.The mixed liquor of getting 2mL is placed in 5mL centrifuge tube, adds the liquor ferri trichloridi of 2mL distilled water and 0.4mL, mixes rapidly.Measure the light absorption value of solution at 700nm place.
Experimental result: see Fig. 1; Testa Phaseoli radiati active component shows good reducing power, shows that Testa Phaseoli radiati active component has potential oxidation resistance.
2, the test of Testa Phaseoli radiati active component to the effect of DPPH free radical scavenging
Experimental principle: DPPH methanol solution is pansy has strong light absorption value under 517nm, if be combined with sample, can reduce light absorption value, removes thus the ability of free radical so as to judgement sample.
Experimental technique
Experimental group: get respectively 0.1mL, 0.2mL, 0.5mL, 1mL Testa Phaseoli radiati active component solution example, in test tube, is supplied 1mL with distilled water, adds 4mLDPPH methanol solution, mixes, and 30min is placed in dark place, constantly concussion, the light absorption value at mensuration 517nm place.
Blank group: get respectively the sample solution of same experimental group equal volume in each test tube, supply 1mL with distilled water, add the methanol solution of 4mL.Mix rear dark place and place 30min, measure 517nm place light absorption value.
Matched group: 1mL distilled water adds 4mLDPPH methanol solution.Mix rear dark place and place 30min, measure the light absorption value at 517nm place.
Experimental result: DPPH suppression ratio (%)=(A0-A1+A2)/A0*100%
The light absorption value that wherein A0 is matched group, the light absorption value that A1 is experimental group, A2 is the light absorption value of corresponding blank group.
The results are shown in Figure 2; Sample can effectively be removed DPPH free radical, and all reaches more than 90% in test specification clearance rate.
3, the scavenging action test of Testa Phaseoli radiati active component to superoxide anion
Experimental principle: pyrogallol autoxidation in weakly alkaline environment decomposes generation superoxide anion, along with the carrying out of reaction, superoxide anion is constantly accumulation in system, cause reactant liquor can linearity increase along with the variation of time in reaction starts a period of time at the absorbance at 420nm place, therefore be determined at the absorbance rate over time of measured object reactant liquor in this period, and more just can show that with blank solution measured object suppresses the ability of superoxide anion.
Experimental technique
Experimental group: get 5.6mLTris HCl buffer, add respectively the testing sample of 0.1mL, 0.2mL, 0.3mL, 0.4mL, supply 0.4mL with distilled water, put into 25 DEG C of water-bath water-bath 10min, then add the pyrogallol (if room temperature can at room temperature operate higher than 25 DEG C) of 25 DEG C of pre-temperature, fully mix, from adding pyrogallol, start accurate timing 3min, then add 5% ascorbic acid (Vc) 0.05mL cessation reaction.After 10min clock, measure its absorbance at 420nm place.
Matched group: get the Tris HCl buffer of 5.6mL, add respectively the testing sample of same experimental group same volume, supply 0.4mL with distilled water, add 12mmol/LHCl, fully mix, from adding HCl to start accurate timing 3min, add 5% ascorbic acid cessation reaction.After 10min clock, measure its absorbance at 420nm place.
Blank group: get 5.6mL50mmol/L Tris-HCl buffer, add 0.4mL distilled water, after this operate same experimental group.
Experimental result: E=[(A0-A1+A2)/A0] * 100%
A0 is blank absorbency value, and A1 is experimental group absorbance, and A2 is matched group absorbance.
The results are shown in Figure 3; Testing sample Testa Phaseoli radiati active component shows the effect of certain removing superoxide anion.
4, copper ion sequestering power test
Experimental principle: metal ion plays the effect of catalyst as iron ion, copper ion in lipid oxidation, cellular oxidation and melanic generative process, the material with metal-chelating effect also can play the effect of antioxidation and check melanin generation indirectly, adopts TMM chelating method to measure copper ion sequestering power with assessment sample chelated mineral ability.
Experimental technique
Standard curve: get respectively 0mL, 0.2mL, 0.4mL, 0.6mL, 0.8mL, the 0.2mM anhydrous slufuric acid copper solution of 1mL, supplies 1mL surely with Hex buffer.Add Hex buffer and the 0.2mLTMM indicator of 4mL, mix and leave standstill 10min, the zeroing of Hex buffer, the light absorption value at mensuration 460nm place and 530nm place.Taking A460/A530 as vertical coordinate, copper ion concentration is abscissa drawing standard curve.
Experimental group: get respectively 0.1mL, 0.2mL, 0.3mL, 0.4mL, 0.5mL sample, in centrifuge tube, is supplied 0.5mL with distilled water, adds 1.5mLHex buffer and 0.5mL to be dissolved in the CuSO of Hex buffer
4(2mM), under room temperature, place 1h, n.s blank is done same processing, separately gets the sample of series of identical volume in centrifuge tube, supplies 0.5mL with distilled water, adds 1mLHex buffer, under room temperature, places 1h.
Get above-mentioned reactant liquor 0.2mL, add 4.8mLHex buffer and 0.2mLTMM indicator, mix and leave standstill 10min, do blank zeroing with Hex buffer, measure the light absorption value at 460nm and 530nm place.
Experimental result: E%=[(A0-A1+A3)/A0] * 100%
A0 is the x value of the blank A460/A530 of n.s correspondence on standard curve, and A1 is experimental group sample A460/A530, and A2 is without copper contrast A460/A530.
The results are shown in Figure 4: sample Testa Phaseoli radiati active component shows stable copper ion sequestering power.
5, Testa Phaseoli radiati active component and the research of Semen phaseoli radiati seed active component to the effect of DPPH free radical scavenging
Experimental technique
Experimental group: get respectively Testa Phaseoli radiati active component solution and prepare Semen phaseoli radiati seed active component solution 1mL prepared by the identical preparation method of Testa Phaseoli radiati active component with using, with distilled water standardize solution to 25mL, therefrom get respectively 1mL solution in test tube, add 4mLDPPH methanol solution, mix, 30min is placed in dark place, constantly concussion, the light absorption value at mensuration 517nm place.
Blank group: get respectively the sample solution of same experimental group equal volume in each test tube, supply 1mL with distilled water, add the methanol solution of 4mL.Mix rear dark place and place 30min, measure 517nm place light absorption value.
Matched group: 1mL distilled water adds 4mLDPPH methanol solution.Mix rear dark place and place 30min, measure the light absorption value at 517nm place.
Experimental result: DPPH suppression ratio (%)=(A0-A1+A2)/A0*100%
See Fig. 5, result shows that the antioxidant effect of Testa Phaseoli radiati active component is better than Semen phaseoli radiati seed active component.
Finally it should be noted that, above embodiment is the unrestricted technical scheme of the present invention in order to explanation only, although the present invention is had been described in detail with reference to above-described embodiment, those skilled in the art are to be understood that, still can modify or be equal to replacement the present invention, and not departing from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in claim scope of the present invention.
Claims (10)
1. a preparation method for Testa Phaseoli radiati active component, is characterized in that, comprises the following steps:
A, get Testa Phaseoli radiati, extracting in water, filters, concentrated, and thin up filters, and obtains sample solution;
B, by after HPD450 absorption with macroporous adsorbent resin on described sample solution, first wash with water to colourless, and then with ethanol elution, obtain eluent, filter, concentrated, obtain Testa Phaseoli radiati active component.
2. the preparation method of Testa Phaseoli radiati active component according to claim 1, is characterized in that: the number of times extracting in described step a is 1～3 time, and the time of extraction is 1～3 hour.
3. the preparation method of Testa Phaseoli radiati active component according to claim 1, is characterized in that: in described step a when extracting in water, the weight adding water is described Testa Phaseoli radiati 8～20 times.
4. the preparation method of Testa Phaseoli radiati active component according to claim 1, is characterized in that: the concentrated concentrating under reduced pressure that adopts in described step a.
5. the preparation method of Testa Phaseoli radiati active component according to claim 1, is characterized in that: in described step a, being concentrated into proportion is 1.05～1.075.
6. the preparation method of Testa Phaseoli radiati active component according to claim 1, is characterized in that: in described step b, the mass percent concentration of ethanol is 70%～90%.
7. the preparation method of Testa Phaseoli radiati active component according to claim 1, is characterized in that: in described step b, being concentrated into proportion is 1.15～1.175.
8. the Testa Phaseoli radiati active component making based on preparation method described in any one in claim 1-7.
9. Testa Phaseoli radiati active component according to claim 8 is in the application of preparing in antioxidation cosmetic product.
10. a cosmetic composition with anti-oxidation function that utilizes the Testa Phaseoli radiati active component described in claim 8 to make, it is characterized in that: this cosmetic composition is composed of the following components: by weight, 1,600～800 parts of 3-butanediols, 50～150 parts of Testa Phaseoli radiati active components, 200～400 parts of purified water, 0.005～0.015 part of phenoxyethanol.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107625672A (en) * | 2016-07-14 | 2018-01-26 | 中国农业科学院作物科学研究所 | A kind of method and application for extracting plurality of active ingredients simultaneously from green gram spermoderm |
| CN115089529A (en) * | 2022-08-03 | 2022-09-23 | 肽源（广州）生物科技有限公司 | Mung bean hull fermentation product with acne removing effect and preparation method and application thereof |
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2014
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Non-Patent Citations (1)
| Title |
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| 陈婷婷等: "绿豆皮中黄酮类化合物提取工艺", 《生物加工过程》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107625672A (en) * | 2016-07-14 | 2018-01-26 | 中国农业科学院作物科学研究所 | A kind of method and application for extracting plurality of active ingredients simultaneously from green gram spermoderm |
| CN115089529A (en) * | 2022-08-03 | 2022-09-23 | 肽源（广州）生物科技有限公司 | Mung bean hull fermentation product with acne removing effect and preparation method and application thereof |
| CN115089529B (en) * | 2022-08-03 | 2023-07-25 | 肽源（广州）生物科技有限公司 | Mung bean hull fermentation product with acne removing effect, and preparation method and application thereof |
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