CN107602644A - A kind of method for extracting purple sweet potato anthocyanin and application - Google Patents
A kind of method for extracting purple sweet potato anthocyanin and application Download PDFInfo
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- CN107602644A CN107602644A CN201710767465.3A CN201710767465A CN107602644A CN 107602644 A CN107602644 A CN 107602644A CN 201710767465 A CN201710767465 A CN 201710767465A CN 107602644 A CN107602644 A CN 107602644A
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Abstract
The invention discloses a kind of method for extracting purple sweet potato anthocyanin and application, belong to flower color glycosides extractive technique field.Methods described includes：Using purple potato powder as raw material, the polyglycol solution that concentration of volume percent is 90 95% is added according to 40 50mL/g liquid ratios, in 65 75 DEG C of water-baths, the 85min of ultrasonic extraction 75, supernatant is separated and collected after cooling, obtains purple sweet potato anthocyanin extract solution.The present invention carries out the extraction of purple sweet potato anthocyanin using polyethylene glycol combination ultrasonic technique, advantageously reduces accessory substance, cost-effective, avoids the potential safety hazard brought using toxic reagent, and polyethylene glycol has protection anthocyanin, improves the effect of extraction stability；In addition, using the inventive method, extraction time is shortened, while improves the yield of anthocyanin.The present invention is simple to operate, cost-effective, improves production efficiency, promotes food security, has preferable economic benefit and social benefit.
Description
Technical field
The present invention relates to flower color glycosides extractive technique field, and in particular to it is a kind of extract purple sweet potato anthocyanin method and should
With.
Background technology
Anthocyanin is the main color-generation material being widely present in nature in flower, fruit, seed and the blade of plant, is
A kind of water-soluble natural pigment, belongs to flavone compound.Flower color glycosides has a variety of physiologically actives and pharmacological action, such as anti-
Oxidation activity, antitumor, anti-mutability, liver protection effect, antihyperglycemic etc., have broad application prospects.
Planting range of the purple sweetpotato in China is wide, and cost of material is low, seasonality is weak, and all contains in its pulp and pericarp
There are a large amount of bright natural anthocyanidin.For purple sweet potato anthocyanin rich in structure is acylated, this causes its stability to be higher than it
His natural pigment.There is research to show containing abundant anthocyanin in purple potato, be potential flower color glycosides extraction raw material.Extraction flower
The accessory substance such as material such as starch, cellulose after color glycosides may be used as producing starch, the raw material of purple sweet potato food and applied to change
Industrial and commercial bank's industry etc. is comprehensively utilized, therefore the comprehensive utilization value of purple potato is higher, and development is significant.Because purple potato has exploitation
The raw material advantage of anthocyanin, it is therefore necessary to study efficient, inexpensive and green purple sweet potato anthocyanin extraction process.
Liu Yanjie, open (optimizing research [J] food industry of purple sweet potato anthocyanin extraction process, 2011 (10) such as strong:48-
51.) technique of anthocyanin is extracted in research from purple potato, and using purple sweet potato powder as raw material, anthocyanin is extracted under the conditions of constant temperature oscillation, is led to
Cross response phase method determine optimum extraction process parameter be 63.76 DEG C of Extracting temperature, extractant be the lemon of mass fraction 0.81%
Aqueous acid, solid-liquid ratio 1:26.36.The mathematical modeling established by Responds Surface Methodology between each factor and response, can be with
Intuitively find out the interaction between each factor.
Yang Zhendong (anthocyanins pigment from purple sweet potato optimal extraction technology is studied and its component analysis [J] China flavouring, and 2011.5
(36)) find that ethanol extraction effect is better than Aqua pure extract in the single factor test research of purple sweetpotato extraction process, the extraction after acid adding
Agent extraction efficiency is higher than the extractant of non-acid adding, and with concentration, hydrochloric acid extraction effect is better than citric acid.Using response phase method to purple
The Extraction technique of sweet potato anthocyanin optimizes research, is 80 DEG C, extraction time 74.7min in Extracting temperature, solid-liquid ratio
1:Under conditions of 28.7, anthocyanins pigment from purple sweet potato extraction yield highest, analyzed by HPLC-DAD, have 15 in No. 1 purple sweetpotato of peaceful purple
Component of the kind with anthocyanin characteristic absorption peak.
Traditional solvent extraction method is using ethanol as extractant, and efficiency is higher, but relative cost is higher, and recovery is tired
Difficulty, and a series of accessory substance can be brought, there is potential health hazard.Therefore, in order to rationally efficiently extract purple potato flower
Color glycosides material, need badly provide it is a kind of it is simple to operate, cost is relatively low, recovery rate is high, the extracting method of safe green.
The content of the invention
It is an object of the invention to provide it is a kind of it is simple to operate, cost is cheap, safe green, and can is efficiently from purple potato
The method for extracting anthocyanin.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of method for extracting purple sweet potato anthocyanin, including：Using purple potato powder as raw material, add according to 40-50mL/g liquid ratios
Enter the polyglycol solution that concentration of volume percent is 90-95%, in 65-75 DEG C of water-bath, ultrasonic extraction 75-85min, cooling
After separate and collect supernatant, obtain purple sweet potato anthocyanin extract solution.
The purple potato powder is dried under the conditions of being placed in 60-70 DEG C after being cut into slices by fresh purple potato, is crushed to 80-100 mesh and is made.
The dissolution of anthocyanin is more beneficial for using powder extraction.
The present invention uses molecular weight as extractant of the 200-400 polyethylene glycol as anthocyanin, the poly- second of low molecule amount
Glycol is non-volatile, and goes back original system to acid, alkali, high temperature, high oxidation system and height and have certain stability, can be compared with
Delay the oxidation course of anthocyanin well.
Research of the present invention has shown that polyethylene glycol contributes to anthocyanin dissolution from purple potato.It is main in purple potato tuber extract
Anthocyanin be using cyanidin and paeonidin as the anthocyanin of core, belong to polar compound, because polyethylene glycol
Polarity is particularly suited for extracting anthocyanin greatly.
The present invention has found that liquid ratio, Polyethylene glycol, Extracting temperature, extraction time are to influence in single factor experiment
The principal element of purple sweet potato anthocyanin extraction, using Box-Behnken method optimization optimum extraction processes.
Preferably, described liquid ratio is 44-45mL/g.
The polyglycol solution is the mixture of polyethylene glycol and water, and polyethylene glycol and water have good compatibility, low
Toxicity and cost is low, contributes to potential safety hazard that is cost-effective, and avoiding other toxic reagents from bringing.Use polyglycol solution
After extracting anthocyanin, without further removing solvent, the supernatant for collecting to obtain is used directly for producing.Preferably, institute
The concentration of volume percent for stating polyglycol solution is 91-92%.
Preferably, described bath temperature is 68-70 DEG C.
The ultrasonic frequency is 120W.It is thin that ultrasonic assistant extraction method utilizes ultrasonic cavitation effect to destroy plant
Born of the same parents, improve solvent penetration so that functional components preferably dissolution.
Preferably, the time of the ultrasonic extraction is 78-80min.
After the completion of extraction, separation of solid and liquid is carried out using centrifugation, it is described to be separated into 10000-11000rpm centrifugations 10-15min.
Preferably, the process conditions after being optimized using response phase method, including：Fresh purple potato is cleaned, is cut into thick about
0.3-0.6cm thin slice, dry, crush at a temperature of 60 DEG C, cross 100 mesh sieves and purple potato powder is made, by 44.05mL/g liquid ratios
The polyglycol solution that concentration of volume percent is 91.55% is added, in 69.3 DEG C of waters bath with thermostatic control, ultrasonic extraction 80min is cold
But, 10min is centrifuged with 11000rpm, collects supernatant, obtain purple sweet potato anthocyanin extract solution.
Preparing food as additive present invention also offers the purple sweet potato anthocyanin extract solution as made from the above method, protecting
Application in strong product or cosmetics.
The beneficial effect that the present invention possesses：
(1) present invention carries out the extraction of purple sweet potato anthocyanin using polyethylene glycol combination ultrasonic technique, cost-effective, avoids making
The potential safety hazard brought with toxic reagent, polyethylene glycol have protection anthocyanin, and the effect for improving extraction stability (is protected under low temperature
Three days are deposited, storage rate 80.75%)；In addition, using the inventive method, extraction time is shortened, while improve anthocyanin
Yield.
(2) compared with Orthogonal Method, the present invention is using Box-Behnken Designs (BBD) center combination design model
Responds Surface Methodology, optimization knot is drawn with 4 changed factors, 3 levels and a small amount of experimental group (only 29 groups of experiments) can
Fruit, optimum yields are obtained, while extraction efficiency is improved, the discharge of energy consumption and pollutant is reduced, there is industrial metaplasia
The practical significance of production.
(3) present invention is simple to operate, cost-effective, improves production efficiency, promotes food security, has preferably warp
Benefit of helping and social benefit.
Brief description of the drawings
Fig. 1 is that Polyethylene glycol of the present invention changes on anthocyanin yield influence figure.
Fig. 2 is that liquid ratio of the present invention changes on anthocyanin yield influence figure.
Fig. 3 is that temperature change of the present invention influences to scheme on anthocyanin yield.
Fig. 4 is to change extraction time of the invention that anthocyanin yield is influenceed to scheme.
Fig. 5 is the response surface graphics that Polyethylene glycol of the present invention influences with liquid ratio on anthocyanin yield.
Fig. 6 is the response surface X-Y scheme that Polyethylene glycol of the present invention influences with liquid ratio on anthocyanin yield.
Fig. 7 is the response surface graphics that Polyethylene glycol of the present invention influences with temperature on anthocyanin yield.
Fig. 8 is the response surface X-Y scheme that Polyethylene glycol of the present invention influences with temperature on anthocyanin yield.
Fig. 9 is the response surface graphics that Polyethylene glycol of the present invention influences with extraction time on anthocyanin yield.
Figure 10 is the response surface X-Y scheme that Polyethylene glycol of the present invention influences with extraction time on anthocyanin yield.
Figure 11 is the response surface graphics that liquid ratio of the present invention influences with temperature on anthocyanin yield.
Figure 12 is the response surface X-Y scheme that liquid ratio of the present invention influences with temperature on anthocyanin yield.
Figure 13 is the response surface graphics that liquid ratio of the present invention influences with extraction time on anthocyanin yield.
Figure 14 is the response surface X-Y scheme that liquid ratio of the present invention influences with extraction time on anthocyanin yield.
Figure 15 is the response surface graphics influenceed with temperature on anthocyanin yield extraction time of the invention.
Figure 16 is the response surface X-Y scheme influenceed with temperature on anthocyanin yield extraction time of the invention.
Embodiment
With reference to embodiment, the invention will be further described.
Experimental method used in following embodiments is conventional method unless otherwise specified.Institute in following embodiments
Material, reagent etc., unless otherwise specified, commercially obtain.
Purple potato is purchased from Zhejiang Jiaxing peasant cooperative society, and kind is that mountains and rivers are purple；Drying unit is electric heating blast drier (Shanghai
Laboratory apparatus Co., Ltd., Factory)；Reducing mechanism is Portable high speed Universalpulverizer (Lin great Machinery Co., Ltd.s of Wenling city)；It is super
Sound water bath device is KH5200B types supersonic generator (Kunshan He Chuan ultrasonic instruments Co., Ltd)；Centrifuge is TGL-16M platforms
Formula high speed freezing centrifuge (Hunan Xiang Yi centrifuges Instrument Ltd.)；Spectrophotometer is UV-5800PC UV, visible lights point
Light photometer (Shanghai Yuan Xi Instrument Ltd.).
Embodiment 1
A kind of polyethylene glycol extracting method for being optimized purple sweet potato anthocyanin using response phase method, is comprised the following steps：
(1) sample preparation：
Fresh purple potato is cleaned, thickness about 0.3-0.6cm thin slice is cut on chopping block, is dried at a temperature of 60 DEG C, is crushed,
Cross 100 mesh sieves.5g purple potatos powder sample accurately is weighed in 500mL conical flasks, and volumetric concentration is added by 25-55mL/g liquid ratios
For 65-95% polyglycol solution, in 45-75 DEG C of water bath with thermostatic control, ultrasonic extraction 65-95min, cool down.With 11000rpm from
Heart 10min, supernatant is collected, obtain the extract solution corresponding to various extracting conditions.
(2) pH shows Anthocyanin content in poor method measure extract solution
1. the preparation of cushioning liquid：
PH1.0 cushioning liquid：It is accurate to prepare 0.2mol/L hydrochloric acid solutions, 0.2mol/L Klorvess Liquids, with hydrochloric acid solution：
Klorvess Liquid=67:25 ratio mixing, it is 1.0 that its pH is adjusted after mixing, and it is standby to be placed in 4 DEG C of refrigerators.
PH4.5 cushioning liquid：The accurate hydrochloric acid solution for preparing 1mol/L, 1mol/L sodium acetate solution are molten with sodium acetate
Liquid：Hydrochloric acid solution：Deionized water=100:60:90 ratio mixing, it is 4.5 that its pH is adjusted after mixing, and it is standby to be placed in 4 DEG C of refrigerators
With.
2. the measure of anthocyanin content in sample：
Anthocyanin crude extract 1.00mL is taken, four times is diluted with pH 1.0 and 4.5 buffer solution respectively, mixes.Room temperature lucifuge
After balancing 30min, absorbance of two kinds of solution at 700nm and 530nm wavelength is determined respectively.Each sample is parallel 3 times, makes even
Average.Anthocyanin yield is calculated as follows, anthocyanin yield is represented with corn flower -3- glucosides.
In formula：A=(A510-A700)pH1.0-(A510-A700)pH4.5；V-extract solution cumulative volume (mL)；N-extension rate；
M-Cy-3-Glu (corn flower -3- glucosides) relative molecular mass (499.2)；ε-Cy-3-Glu extinction coefficient
(29600)；M-sample quality (g).
(3) experimental design and statistical analysis：
1. single factor experiment：
Change Polyethylene glycol, liquid ratio, temperature, extraction time progress single factor experiment successively, show that poor method is surveyed with pH
Anthocyanin yield in fixed gained purple sweet potato anthocyanin extract.
As Figure 1-4, extraction yield of the 4 above-mentioned factors on purple sweet potato anthocyanin influences more significant.
2. response phase method optimization design：
According to single factor experiment result, it is suitable to choose four Polyethylene glycol, liquid ratio, temperature, extraction time factors
Zero level, using the softwares of Design Expert 8.0 according to Box-Behnken design principles carry out experimental design (setting tie
1) fruit is shown in Table, with Polyethylene glycol X1, liquid ratio X2, temperature X3, extraction time X4For independent variable, using anthocyanin yield to ring
Should value y (experimental program and the results are shown in Table 2), establish polynary quadratic regression equation：
Y=82.95+3.95X1+0.50X2+2.56X3-0.71X4+0.43X1X2+6.53X1X3-0.92X1X4+2.42X2X3+
2.27X2X4+1.29X3X4-15.15X1 2-4.38X2 2-6.64X3 2-4.04X4 2。
Linear relationship conspicuousness between each factor and response, examined and judged by F values, P values are smaller, then explanatory variable
Conspicuousness is higher.From analysis of variance table (table 3), the linear relationship significantly (R between its dependent variable and all independents variable2=
0.9248), the model level of signifiance is less than 0.05, so the regression equation model is significant.
The empirical factor of table 1 and level set
Table 2Box-Behnken experimental designs and result
The results of analysis of variance of the experimental data of table 3
Note:* significant difference, p are represented<0.05；* represents that difference is extremely notable, p<0.01.
(4) analysis of experimental results and optimization：
Plot analysis is carried out according to polynary quadratic regression equation using the softwares of Design Expert 8.0, obtains recurrence side
The response surface and its contour map (such as Fig. 5-16) of journey.
The optimum extraction condition that purple sweet potato anthocyanin is obtained by the softwares of Design Expert 8.0 is：Polyethylene glycol is
91.55%, liquid ratio 44.05mL/g, temperature are 69.3 DEG C, extraction time 80min, on this condition, anthocyanin yield
Predicted value is 79.43mg/100g.
Embodiment 2
Fresh purple potato is cleaned, thickness about 0.3-0.6cm thin slice is cut on chopping block, is dried at a temperature of 60 DEG C, is crushed,
Cross 100 mesh sieves.
5g purple potatos powder sample accurately is weighed in 500mL conical flasks, and percent by volume is added by 44.05mL/g liquid ratios
Concentration is 91.55% polyglycol solution, in 69.3 DEG C of waters bath with thermostatic control, ultrasonic extraction 80min, and cooling.With 11000rpm from
Heart 10min, supernatant is collected, obtains purple sweet potato anthocyanin extract solution.
PH shows Anthocyanin content in poor method measure extract solution, and anthocyanin yield actual value is 78.01mg/100g, and pre-
Measured value is close, illustrates that the extraction conditions of optimization gained are reliable.
Embodiment 3
Fresh purple potato is cleaned, thickness about 0.3-0.6cm thin slice is cut on chopping block, is dried at a temperature of 60 DEG C, is crushed,
Cross 100 mesh sieves.
5g purple potatos powder sample accurately is weighed in 500mL conical flasks, and it is dense to add percent by volume by 40mL/g liquid ratios
The polyglycol solution for 90% is spent, in 65 DEG C of waters bath with thermostatic control, ultrasonic extraction 75min, cooling.10min is centrifuged with 11000rpm,
Supernatant is collected, obtains purple sweet potato anthocyanin extract solution.
PH shows Anthocyanin content in poor method measure extract solution, and anthocyanin yield actual value is 76.54mg/100g.
Embodiment 4
Fresh purple potato is cleaned, thickness about 0.3-0.6cm thin slice is cut on chopping block, is dried at a temperature of 60 DEG C, is crushed,
Cross 100 mesh sieves.
5g purple potatos powder sample accurately is weighed in 500mL conical flasks, and it is dense to add percent by volume by 50mL/g liquid ratios
The polyglycol solution for 95% is spent, in 75 DEG C of waters bath with thermostatic control, ultrasonic extraction 85min, cooling.10min is centrifuged with 11000rpm,
Supernatant is collected, obtains purple sweet potato anthocyanin extract solution.
PH shows Anthocyanin content in poor method measure extract solution, and anthocyanin yield actual value is 77.23mg/100g.
Embodiment 5
Fresh purple potato is cleaned, thickness about 0.3-0.6cm thin slice is cut on chopping block, is dried at a temperature of 60 DEG C, is crushed,
Cross 100 mesh sieves.
5g purple potatos powder sample accurately is weighed in 500mL conical flasks, and it is dense to add percent by volume by 45mL/g liquid ratios
The polyglycol solution for 92% is spent, in 70 DEG C of waters bath with thermostatic control, ultrasonic extraction 80min, cooling.10min is centrifuged with 11000rpm,
Supernatant is collected, obtains purple sweet potato anthocyanin extract solution.
PH shows Anthocyanin content in poor method measure extract solution, and anthocyanin yield actual value is 77.61mg/100g.
Comparative example 1
Using (Liu Yanjie, optimizing research [J] food industry of a strong purple sweet potato anthocyanin extraction process, 2011 (10):
48-51.) the optimization method of report, 63.76 DEG C of Extracting temperature, citric acid mass fraction 0.81%, solid-liquid ratio 1: 26.36 are carried out
Contrast test is extracted, gained anthocyanin yield is 71.08mg/100g.Carried using the anthocyanin yield of the method for embodiment 2 compared to it
It is high by nearly 9%.
Comparative example 2
The extraction process of parameter embodiment 2, wherein extractant polyglycol solution are substituted for concentration of volume percent and are
91.55% ethanol solution, gained anthocyanin yield are 77.32mg/100g, are approached with this method anthocyanin yield, further
Prove that the extraction effect of this method is good.
Application examples
The final purpose of present invention extraction purple sweet potato anthocyanin is exactly to use it in daily production, so as to play its biology
Function.Therefore, the present invention proposes a kind of mode of production that extract solution is directly used in food or cosmetics.
Polyethylene glycol may be directly applied to reality as the important composition composition in numerous food product, medicine and cosmetics
Production in.Solvent step is removed this not only reduces traditional ethanol extraction method, greatlys save production cost, and meet
The Production trend of green energy conservation, avoid unnecessary emission.
By taking candy common on the market, capsule for medicine and lipstick as an example, the general formula of candy is glucose syrup, white sand
Sugar, edible fruit glaze agent (polyethylene glycol)；The general formula of capsule for medicine be starch, edible fruit glaze agent (polyethylene glycol) and some
Medicinal ingredient；The general formula of lipstick is fruit oil, hydrogenated rosins acid methyl esters, polyethylene glycol and some functional component (vitamins
E) etc..The anthocyanin contained by polyethylene glycol extract that present invention extraction obtains has many physiological functions such as anti-oxidant, can
Strengthen the feature of above-mentioned food, medicine and cosmetics, widen the market of product, attract more consumers.As can be seen here, this hair
Bright using extraction solution polyethylene glycol is important food, medicine and Cosmetic Manufacture raw material, possess be directly used in production can
Energy.
The present invention for purple sweet potato anthocyanin, further lay a good foundation by research and integrated application.
Claims (10)
- A kind of 1. method for extracting purple sweet potato anthocyanin, it is characterised in that including：Using purple potato powder as raw material, according to 40-50mL/g Liquid ratio adds the polyglycol solution that concentration of volume percent is 90-95%, in 65-75 DEG C of water-bath, ultrasonic extraction 75- 85min, supernatant is separated and collected after cooling, obtain purple sweet potato anthocyanin extract solution.
- 2. the method as described in claim 1, it is characterised in that the purple potato powder is placed in 60-70 after being cut into slices by fresh purple potato Dried under the conditions of DEG C, be crushed to 80-100 mesh and be made.
- 3. the method as described in claim 1, it is characterised in that described liquid ratio is 44-45mL/g.
- 4. the method as described in claim 1, it is characterised in that the molecular weight of the polyethylene glycol is 200-400.
- 5. the method as described in claim 1, it is characterised in that the concentration of volume percent of the polyglycol solution is 91- 92%.
- 6. the method as described in claim 1, it is characterised in that described bath temperature is 68-70 DEG C.
- 7. the method as described in claim 1, it is characterised in that the ultrasonic frequency is 120W.
- 8. method as claimed in claim 7, it is characterised in that the time of the ultrasonic extraction is 78-80min.
- 9. the method as described in claim 1, it is characterised in that the process conditions after being optimized using response phase method, including：Will be new Light violet potato is cleaned, and is cut into thickness about 0.3-0.6cm thin slice, is dried at a temperature of 60 DEG C, is crushed, and crosses 100 mesh sieves and purple sweet potato powder is made End, the polyglycol solution that concentration of volume percent is 91.55%, 69.3 DEG C of waters bath with thermostatic control are added by 44.05mL/g liquid ratios In, ultrasonic extraction 80min, cooling, 10min is centrifuged with 11000rpm, supernatant is collected, obtains purple sweet potato anthocyanin extract solution.
- 10. the purple sweet potato anthocyanin extract solution as made from any one of claim 1-9 methods described as additive prepare food, Application in health products or cosmetics.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109090577A (en) * | 2018-10-16 | 2018-12-28 | 安徽祥康生物工程有限公司 | A kind of Cordyceps militaris meal replacement powder and its preparation method |
| CN113372400A (en) * | 2021-06-09 | 2021-09-10 | 贵州侗乡生态农业科技发展有限公司 | Method for extracting anthocyanin from perilla leaves |
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| CN103665072A (en) * | 2012-09-07 | 2014-03-26 | 合肥师范学院 | Extraction method of purple sweet potato anthocyanin |
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| CN103665072A (en) * | 2012-09-07 | 2014-03-26 | 合肥师范学院 | Extraction method of purple sweet potato anthocyanin |
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| CN109090577A (en) * | 2018-10-16 | 2018-12-28 | 安徽祥康生物工程有限公司 | A kind of Cordyceps militaris meal replacement powder and its preparation method |
| CN113372400A (en) * | 2021-06-09 | 2021-09-10 | 贵州侗乡生态农业科技发展有限公司 | Method for extracting anthocyanin from perilla leaves |
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