CN104098925A - Method for rapidly extracting antioxidative purple sweet potato pigment - Google Patents
Method for rapidly extracting antioxidative purple sweet potato pigment Download PDFInfo
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- CN104098925A CN104098925A CN201410369679.1A CN201410369679A CN104098925A CN 104098925 A CN104098925 A CN 104098925A CN 201410369679 A CN201410369679 A CN 201410369679A CN 104098925 A CN104098925 A CN 104098925A
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- dioscoreae esculentae
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Abstract
The invention discloses a method for rapidly extracting antioxidative purple sweet potato pigment, which comprises the specific steps as follows: a, washing fresh purple sweet potatoes, cutting the fresh purple sweet potatoes into small cubes, drying the small cubes in a blast drying oven, and then smashing the dried small cubes into powder in an agitator; b, using a rapid solvent extraction device to extract the powder obtained in step a; c, performing centrifugal filtration on the extractant obtained in step b to obtain a supernate, and concentrating the supernate under reduced pressure. According to the invention, the pigment extraction ratio is increased, the extraction time is shortened, and the pigment extracted and obtained through the method has a higher antioxidative efficacy.
Description
Technical field
The present invention relates to food, medicine, makeup preparation field, relate in particular to a kind of natural pigment extracting method.
Background technology
Anthocyanidin is progressively subject to popular concern and attention in recent decades, have the more and more product about anthocyanidin to come out in fields such as food, medicine, makeup.In food, anthocyanidin can be used as a kind of tinting material, makes product present needed color, and Nantural non-toxic.
Rhizoma Dioscoreae esculentae, formal name used at school ginseng potato, has another name called black potato, and potato meat is that purple is to intense violet color.Because be rich in anthocyania pigment, become in recent years a kind of increasingly popular foodstuff raw material with coming into one's own.Also in rising trend about extracting the research topic of Rhizoma Dioscoreae esculentae anthocyanidin.
The extracting method of anthocyanidin mainly contains traditional water bath method, supersonic method, quick solvent extraction instrument method, high hydrostatic pressure method, pulsed electrical field method, microwave extraction method, supercritical fluid extraction, solid phase extraction, ion-exchange back extraction method etc.
Wherein, traditional water bath method (CN103160139A, CN102020868A, CN103193839A, CN102675912A), ultrasonic extraction (CN101530191), microwave extraction method (Liu Jie, leaf is graceful. and enzyme-microwave-assisted extracts the technical study [J] of purple potato anthocyanidin. Chemical Industry in Guangzhou, 2012,40:60-62; Xu Zhenghong, Gao Yanxiang, Shi Sulan, etc. the research [J] of Extraction of Pigment from Purple Sweet Potato Powder by Microwave-assisted Technique. Food science, 2005,26:234-238) etc. method, sometimes aid in enzymolysis process (CN102020868A; CN101530191, CN103193839A), for the extracting and preparing technique of Rhizoma Dioscoreae esculentae.
Traditional water bath extraction method is the inorganic or organic solvent that conventionally adopts acidifying, the mixture of sample and solvent is put into and is stirred, thereby reach the object of extracting anthocyanidin.The method simply still has the drawback that relative extraction time is long, solvent usage quantity is large.
Ultrasonic extraction, by the cell walls of the broken plant tissue of hyperacoustic oscillation action, flows out in solvent anthocyanidin material, can greatly shorten extraction time.The application of ultrasonic extraction mass-producing in foodstuffs industry.
Microwave extraction method is to utilize microwave heating to make the fast rise of vegetable cell temperature, when liquid water in cell is vaporized, produce larger pressure, cytolemma and cell walls can be broken through, solvent is easy to enter in cell, dissolve and discharge coloring matter, impel it to be comparatively fast extracted.But the temperature of microwave heating is higher, may cause the anthocyanidin degraded of thermolability.
Therefore, those skilled in the art is devoted to develop a kind of method of utilizing the condition of high pressure, short time high temperature Rhizoma Dioscoreae esculentae to be extracted fast to extraction pigment.
Summary of the invention
Because the above-mentioned defect of prior art, technical problem to be solved by this invention is how to improve the productive rate of Ipomoea batatas(L.)Lam material, shortens extraction time, improves the antioxidant effect of coloring matter simultaneously.
For achieving the above object, the invention provides a kind of method of utilizing quick solvent extraction instrument to extract Ipomoea batatas(L.)Lam.Concrete steps are as follows:
A. fresh Rhizoma Dioscoreae esculentae is cleaned, be cut into Rhizoma Dioscoreae esculentae fourth, put into air dry oven oven dry, then put into stirrer and blend into powder;
B. utilize quick solvent extraction instrument to extract the powder obtaining in step a;
C. extract step b being obtained carries out centrifuging, obtains supernatant liquor, by supernatant liquor concentrating under reduced pressure.
Preferably, the particle diameter of the Rhizoma Dioscoreae esculentae fourth in step a is 2-3mm; Rhizoma Dioscoreae esculentae fourth is dried to moisture content < 20% in air dry oven; The fineness that purple potato fourth is blended into powder is 20-40 order.
Preferably, 95% ethanol that the solvent using in step b is acidifying, wherein contains volume ratio and is 0.1% concentrated hydrochloric acid; Solid-liquid ratio is 1:20 (g:mL).
In the step b of above-mentioned condition, preferred extraction temperature scope is 60-120 DEG C, and the preferred static extracting time is 5-30min, and preferred cycle index is 1-3 time.
Preferably, in step c, supernatant liquor is evaporated to below 1/5 of original volume, in order to follow-up use.
The present invention has following advantage and effect with respect to prior art:
(1) the present invention utilizes under the condition of high pressure, short time high temperature, Rhizoma Dioscoreae esculentae is extracted fast with a small amount of organic solvent, improves pigment extraction yield, and shortens extraction time.
(2) the object of the invention is to provide a kind of simple purple potato anthocyania pigment extracting method fast, extracts the coloring matter obtaining have stronger anti-oxidation efficacy through the method.
(3) pigment of preparing through the inventive method, has kept original Rhizoma Dioscoreae esculentae anthocyanidin monomeric substance kind and ratio thereof.
Below with reference to accompanying drawing, the technique effect of design of the present invention, concrete structure and generation is described further, to understand fully object of the present invention, feature and effect.
Brief description of the drawings
Fig. 1 is that the embodiment of the present invention 3 obtains Rhizoma Dioscoreae esculentae anthocyanidin yield comparison diagram with Traditional Method, supersonic method;
Fig. 2 is the Rhizoma Dioscoreae esculentae anthocyanidin monomer HPLC collection of illustrative plates that traditional extraction method obtains.
Fig. 3 is the Rhizoma Dioscoreae esculentae anthocyanidin monomer HPLC collection of illustrative plates that ultrasonic extraction obtains.
Fig. 4 is the Rhizoma Dioscoreae esculentae anthocyanidin monomer HPLC collection of illustrative plates that the embodiment of the present invention 3 obtains.
Fig. 5 is the anti-oxidant activity comparison diagram of the Rhizoma Dioscoreae esculentae anthocyanidin that obtains of the present invention and Traditional Method, supersonic method.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
embodiment 1
Fresh Rhizoma Dioscoreae esculentae is cleaned, be cut into the Rhizoma Dioscoreae esculentae fourth of 2-3mm.Put into air dry oven and be dried to moisture content < 20%, then putting into stirrer, to blend into fineness be 20 object powder.With the extraction of the quick solvent extraction instrument of ASE350, it imposes a condition as: temperature 60 C, static extracting time 30min, cycle index 3 times.Other conditions are: solvent 95% ethanol (concentrated hydrochloric acid that is 0.1% containing volume ratio), the about 1:20 of solid-liquid ratio (g:mL).After extraction completes, centrifuging, obtains supernatant liquor.Supernatant liquor concentrating under reduced pressure is to below 1/5 of original volume, for subsequent use.
embodiment 2
Fresh Rhizoma Dioscoreae esculentae is cleaned, be cut into the Rhizoma Dioscoreae esculentae fourth of 2-3mm.Put into air dry oven and be dried to moisture content < 20%, then putting into stirrer, to blend into fineness be 40 object powder.With the extraction of the quick solvent extraction instrument of ASE350, it imposes a condition as: 120 DEG C of temperature, static extracting time 5min, cycle index 1 time.Other conditions are: solvent 95% ethanol (concentrated hydrochloric acid that is 0.1% containing volume ratio), the about 1:20 of solid-liquid ratio (g:mL).After extraction completes, centrifuging, obtains supernatant liquor.Supernatant liquor concentrating under reduced pressure is to below 1/5 of original volume, for subsequent use.
embodiment 3
Fresh Rhizoma Dioscoreae esculentae is cleaned, be cut into the Rhizoma Dioscoreae esculentae fourth of 2-3mm.Put into air dry oven and be dried to moisture content < 20%, then putting into stirrer, to blend into fineness be 40 order powder.With the extraction of the quick solvent extraction instrument of ASE350, it imposes a condition as: 90 DEG C of temperature, static extracting time 20min, cycle index 2 times.Other conditions are: solvent 95% ethanol (concentrated hydrochloric acid that is 0.1% containing volume ratio), the about 1:20 of solid-liquid ratio (g:mL).After extraction completes, centrifuging, obtains supernatant liquor.Supernatant liquor concentrating under reduced pressure is to below 1/5 of original volume, for subsequent use.
Table 1 is the Ipomoea batatas(L.)Lam yield of solvent extration fast
comparative example 1
Fresh Rhizoma Dioscoreae esculentae is cleaned, be cut into the Rhizoma Dioscoreae esculentae fourth of 2-3mm.Put into air dry oven and be dried to moisture content < 20%, then putting into stirrer, to blend into fineness be 40 order powder.Mix with 80% ethanol (containing volume ratio is 0.01% concentrated hydrochloric acid) of acidifying according to the solid-liquid ratio of 1:20 (g:ml), 70 DEG C of temperature heated and stirred 90 minutes.Then centrifuging, obtains supernatant liquor.Supernatant liquor concentrating under reduced pressure is to below 1/5 of original volume, for subsequent use.
comparative example 2
Fresh Rhizoma Dioscoreae esculentae is cleaned, be cut into the Rhizoma Dioscoreae esculentae fourth of 2-3mm.Put into air dry oven and be dried to moisture content < 20%, then putting into stirrer, to blend into fineness be 40 order powder.Mix with 90% ethanol (containing volume ratio is 0.01% concentrated hydrochloric acid) of acidifying according to the solid-liquid ratio of 1:20 (g:ml), pack in air-tight bottle.Sealed flask is inverted in THC type numerical control supersonic extracting machine, covers extracting machine lid, set corresponding time 45min, ultrasonic power 200W.After extraction completes, centrifuging, obtains supernatant liquor.Supernatant liquor concentrating under reduced pressure is to below 1/5 of original volume, for subsequent use.
contrast experiment and result
PH differential is measured total anthocyanidin content: in a glass cuvette, add 200 μ L samples and 3mL0.025mol/L Repone K-hydrochloric acid buffer solution (pH=1.0); In another glass cuvette, add 200 μ L samples and 3mL 0.4mol/L sodium acetate-acetic acid buffer solution (pH=4.5).Two cuvettes are placed on to dark place, balance 15min.Then two cuvettes are put into spectrophotometer and measured respectively both at 520nm with in the absorbancy at 700nm place, calculate the light absorption value Δ A of the sample after dilution.Its calculation formula is:
ΔA＝(A
520nm-A
700nm)
pH1.0-(A
520nm-A
700nm)
pH4.5
In formula:
W---total anthocyanidin content in sample, the mg/100g of unit dry weight;
Δ A---the light absorption value of sample after dilution;
MW---molecular weight 449.2;
V---be extracting solution cumulative volume (mL);
ε---molar absorptivity 26900 (L mol
-1.cm
-1);
M---the sample quality taking before extraction, the g of unit.
The pigment extract that comparative example 1, comparative example 2 and embodiment 3 are obtained carries out the analysis of anthocyanidin total content, and result as shown in Figure 1.
Use efficient liquid phase chromatographic analysis anthocyanidin: instrument model Surveyor Plus, Thermo company of the U.S..Chromatographic column is that (250mm × 4.6mm, 5 μ m) for C18 post.Column temperature is 25 DEG C.Flow velocity is 1mL/min.Sample size 25 μ L; Wavelength 520nm; Mobile phase A is 1% formic acid-aqueous solution (V/V) mutually, and B is 1% formic acid-acetonitrile solution (V/V) mutually.Gradient elution program is: 0 to 5min 85% (V/V) A phase, and 5 to 30min A change to 80% (V/V) from 85% (V/V), the 30th to 45 min, A drops to 60% (V/V) mutually.The pigment extract that comparative example 1, comparative example 2, embodiment 3 are obtained has carried out anthocyanidin monosomic analysis, and its result corresponds respectively to Fig. 2,3 and 4.
Iron ion reduction method (FRAP, ferric reducing antioxidant power): get the Rhizoma Dioscoreae esculentae extracting solution (embodiment 3 that 6mL FRAP working fluid and 1mL diluted, comparative example 1 and comparative example 2), mix, at 37 DEG C of water bath with thermostatic control 10min, then measure light absorption value at 593nm place.With Trolox standardized solution (10 μ mol/L, 20 μ mol/L, 40 μ mol/L, 60 μ mol/L, 80 μ mol/L) the production standard curve of different concns.Result represents the reducing power of Rhizoma Dioscoreae esculentae extracting solution using Trolox content as equivalent.
The wherein preparation of FRAP working fluid: formulated with the ratio of volume ratio 10:1:1 by 0.3mmol/L pH=3.6 sodium acetate-acetic acid buffer solution, 10mmol/L TPTZ (three pyridine three azines) solution, 20mmol/L ferric chloride Solution.
The pigment extract that comparative example 1, comparative example 2 and embodiment 3 are obtained has carried out reducing power analysis, and result as shown in Figure 5.
Above result shows, within the short period of time (15min), obtain higher anthocyanidin material yield than Traditional Method (90min), the quick solvent extration of supersonic method (45min), and anthocyanidin monomeric substance is almost constant, in addition, the total reducing power of anthocyania pigment is stronger.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that those of ordinary skill in the art just can design according to the present invention make many modifications and variations without creative work.Therefore, all technician in the art, all should be in by the determined protection domain of claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (10)
1. an anti-oxidant Ipomoea batatas(L.)Lam rapid extracting method, is characterized in that, comprises the steps:
A. fresh Rhizoma Dioscoreae esculentae is cleaned, be cut into Rhizoma Dioscoreae esculentae fourth, put into air dry oven oven dry, then put into stirrer and blend into powder;
B. the powder that utilizes quick solvent extraction instrument to obtain step a extracts;
C. extract step b being obtained carries out centrifuging, obtains supernatant liquor, by supernatant liquor concentrating under reduced pressure.
2. the method for claim 1, is characterized in that, the particle diameter of the fourth of Rhizoma Dioscoreae esculentae described in step a is 2-3mm.
3. the method for claim 1, is characterized in that, the described Rhizoma Dioscoreae esculentae fourth in step a is dried to moisture content < 20% in air dry oven.
4. the method for claim 1, is characterized in that, the fineness that the described purple potato fourth in step a is blended into powder is 20-40 order.
5. the method for claim 1, is characterized in that, 95% ethanol that solvent described in step b is acidifying wherein contains volume ratio and be 0.1% concentrated hydrochloric acid.
6. method as claimed in claim 5, is characterized in that, the solid-liquid ratio extracting described in step b is 1:20 (g:mL).
7. the method as described in claim 5 or 6, is characterized in that, the temperature range extracting described in step b is 60-120 DEG C.
8. the method as described in claim 5 or 6, is characterized in that, the static extracting time extracting described in step b is 5-30min.
9. the method as described in claim 5 or 6, is characterized in that, the cycle index extracting described in step b is 1-3 time.
10. the method as described in claim 1-6 any one, is characterized in that, described in step c, supernatant liquor concentrating under reduced pressure is referred to and is concentrated into below 1/5 of original volume.
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Cited By (5)
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| CN104644720A (en) * | 2015-02-02 | 2015-05-27 | 河南大学 | Purple sweet potato extract as well as preparation method and application thereof |
| CN105092500A (en) * | 2015-09-22 | 2015-11-25 | 江苏农林职业技术学院 | Method for determining grape anthocyanin content easily, conveniently and rapidly |
| CN108936151A (en) * | 2018-06-04 | 2018-12-07 | 天津商业大学 | A kind of compound antianxiety sleeping drink of black fruit fructus lycii and preparation method thereof |
| CN109233326A (en) * | 2018-09-11 | 2019-01-18 | 泉州市缘创环保科技有限公司 | A kind of colouring method of natural Ipomoea batatas(L.)Lam |
| CN110022675A (en) * | 2016-10-05 | 2019-07-16 | 三荣源有限公司 | The method of coloured sweet potato, its converted products and its determining kind with high anthocyanidin content |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN110022675A (en) * | 2016-10-05 | 2019-07-16 | 三荣源有限公司 | The method of coloured sweet potato, its converted products and its determining kind with high anthocyanidin content |
| CN108936151A (en) * | 2018-06-04 | 2018-12-07 | 天津商业大学 | A kind of compound antianxiety sleeping drink of black fruit fructus lycii and preparation method thereof |
| CN109233326A (en) * | 2018-09-11 | 2019-01-18 | 泉州市缘创环保科技有限公司 | A kind of colouring method of natural Ipomoea batatas(L.)Lam |
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