CN102172364B - Method for extracting general flavone from peas in ultrasound-assisted way - Google Patents
Method for extracting general flavone from peas in ultrasound-assisted way Download PDFInfo
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- CN102172364B CN102172364B CN 201110053244 CN201110053244A CN102172364B CN 102172364 B CN102172364 B CN 102172364B CN 201110053244 CN201110053244 CN 201110053244 CN 201110053244 A CN201110053244 A CN 201110053244A CN 102172364 B CN102172364 B CN 102172364B
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Abstract
The invention discloses a method for extracting general flavone from peas in an ultrasound-assisted way. The method comprises the following steps of: (1) drying peas, smashing, screening, making the screened pea flour reflow with petroleum ether to remove lipid and pigments and putting the reflowed pea flour into a constant-temperature drying box for drying to obtain treated pea flour; (2) mixing the treated pea flour obtained in the step (1) with an ethanol solution in the solution-flour ratio of (10:1)-(50:1), ultrasonically extracting under the condition that the temperature is 50-90 DEG C, the ultrasonic power is 200-600 W and the pH value is 2-10 for 20-60 minutes to obtain a general flavone extracting solution, centrifuging the extracting solution at the speed of 10,000 revolutions per minute for 10 minutes, and leaching to obtain a general flavone ethanol-water solution, wherein the volume fraction of ethanol in the ethanol solution is 20-80 percent; and removing the ethanol from the general flavone ethanol-water solution by performing rotary evaporation, and performing freeze drying with a vacuum freeze drier to obtain general flavone powder. Compared with the conventional extracting method, the method has the advantages of short extracting time, high yield and the like; and moreover, the ultrasonic extraction is a physical process without any chemical reaction, so that the changes of bioactive substances are reduced.
Description
Technical field
The present invention relates to a kind of method of extracting the pea total flavones, especially a kind of method of extracting general flavone from peas in ultrasound-assisted way.
Background technology
The extraction of pea total flavones method commonly used is solvent-extraction process at present, and solvent-extraction process comprises hot water extraction method and organic solvent extraction method.The hot water extraction method only can be used for extracting the chromocor compound of strong polarity, and it is low to extract yield, and extraction time is long, solvent consumption is large; The impurity such as the protein carbohydrate of hot water extraction stripping are many, the difficulty that has increased for follow-up process for refining.Organic solvent method extraction time is long, solvent load is large; The product residue organic solvent that extracts is unfavorable for the food service industry application; The Enzymatic Extraction selectivity is better, but cost is high, and yield is lower.
In addition: extract at present method of design and mainly concentrate on and carry out orthogonal optimization, although it has a lot of superiority than experiment of single factor commonly used, experiment number obviously reduces; Can by variance analysis, obtain secondary factors that affects experimental result etc.But owing to often having interaction between factor, so that being total energy, orthogonal method do not obtain best optimal conditions.Orthogonal Optimization can only be processed discrete horizontal factor, obtain that prioritization scheme then need to be by experience more specifically.
Response Surface Method (response surface methodology, RSM) be a kind of optimum experimental method, not only can set up the continuous variable surface model, also can estimate the factor and interaction thereof, can do regression analysis to concentrating factor interaction, the optimization data that obtains is more approaching effectively more near true horizon, thereby more with practical value.The three-dimensional picture that response surface analysis obtains can must find out very intuitively that each factor is on the impact of experimental result.
Summary of the invention
Technical problem to be solved by this invention is to provide for the existing problem of the solvent-extraction process of above-mentioned pea total flavones a kind of method of extracting general flavone from peas in ultrasound-assisted way, the method is compared with conventional extraction method, and it has short, productive rate advantages of higher of extraction time; And supersound extraction is a physical process, therebetween without chemical reaction, reduced the change of biologically active substance.
Technical problem to be solved by this invention can be achieved through the following technical solutions:
A kind of method of extracting general flavone from peas in ultrasound-assisted way comprises the steps:
(1) processing of bean powder
Pea is dried to water ratio≤5%, put into medicinal herb grinder and pulverize, sieve; Bean powder after sieving refluxes with sherwood oil and removes lipid and pigment, and the bean powder after then will refluxing is dried the bean powder that must handle well to water ratio≤3% as for thermostatic drying chamber;
(2) extract
The bean powder that step (1) is handled well and ethanolic soln are to mix in 10: 1～50: 1 by liquid ratio, volume grade of alcohol is 20～80% in the ethanolic soln, it is 50～90 ℃ in temperature, ultrasonic power is 200～600W, the pH value is that 2～10 condition supersound extraction obtained the total flavones extracting solution in 20～60 minutes, extracting solution obtains general flavone ethanol-aqueous solution through centrifugal 10 minutes of 10000r/min suction filtration then.General flavone ethanol-aqueous solution is removed ethanol through rotary evaporation, then obtains the total flavones powder with the vacuum freeze drier drying.
In a preferred embodiment of the invention, in the described step (2), volume grade of alcohol is preferably 65% in the ethanolic soln.
In a preferred embodiment of the invention, in the described step (2), its pH value is preferably 8.
In a preferred embodiment of the invention, in the described step (2), the supersound extraction time is preferably 30 minutes.
In a preferred embodiment of the invention, in the described step (2), ultrasonic power is preferably 500W.
In a preferred embodiment of the invention, in the described step (2), liquid ratio is preferably 20: 1.
In a preferred embodiment of the invention, in the described step (2), temperature is preferably 60 ℃.
In a preferred embodiment of the invention, in the described step (2), described solid-liquid ratio is preferably 20.80: 1, and temperature is preferably 60.86 ℃, and volume fraction of ethanol is preferably 63.58%.
Access method of the present invention has short, productive rate advantages of higher of extraction time; And supersound extraction is a physical process, therebetween without chemical reaction, reduced the change of biologically active substance.
Embodiment
The following examples can help the present invention of those skilled in the art comprehend, but do not limit the present invention in any way.
A kind of method of extracting general flavone from peas in ultrasound-assisted way comprises the steps:
1, the preparation of bean powder
Pea in 80 ℃ of thermostatic drying chamber oven dry 3 hours, is put into medicinal herb grinder and pulverized, cross 80 mesh sieves for subsequent use.Bean powder after sieving refluxes with sherwood oil and removed lipid and pigment in 2 hours, the bean powder that the bean powder after then will refluxing must be handled well as for 80 ℃ of oven dry of thermostatic drying chamber in 3 hours.
2, extract
The bean powder that step (1) is handled well and ethanolic soln are to mix in 10: 1～50: 1 by liquid ratio, volume grade of alcohol is 20～80% in the ethanolic soln, it is 50～90 ℃ in temperature, ultrasonic power is 200～600W, the pH value is that 2～10 condition supersound extraction obtained the total flavones extracting solution in 20～60 minutes, extracting solution obtains general flavone ethanol-aqueous solution through centrifugal 10 minutes of 10000r/min suction filtration then.General flavone ethanol-aqueous solution is removed ethanol through rotary evaporation, then obtains the total flavones powder with the vacuum freeze drier drying.
Below by single factor experiment method and Response surface methodology ultrasonic power, extraction temperature, extraction time, volume fraction of ethanol, liquid ratio are tested the impact of extracting yield, with ultrasonic power, extraction temperature, extraction time, volume fraction of ethanol, the liquid ratio of choosing optimization.
1, single factor experiment comprises: ultrasonic power, extraction temperature, extraction time, volume fraction of ethanol, liquid ratio are on extracting the impact of yield.Specific implementation method sees Table 1
Table 1 single factor experiment is investigated factor and level
2, the response curved surface is optimized extraction conditions
Adopt Response Surface Method research to extract temperature, liquid ratio, volume fraction of ethanol and liquid ratio are extracted yield on the pea total flavones impact.Specific implementation method sees Table 2
Table 2 response surface experimental factor and level
Test-results:
A: volume fraction of ethanol is on extracting the impact of yield
Be under the condition of 600W at liquid ratio 20: 1,80 ℃ of temperature, time 20min, ultrasonic power, investigate volume fraction of ethanol extracts yield on the pea total flavones in 20%, 35%, 50%, 65%, 80% scope impact, the result shows that the extraction using alcohol gained extraction yield with 65% is the highest.
The b:pH value is on extracting the impact of yield
Under the condition of liquid ratio 20: 1, extraction temperature 60 C, extraction time 30min, volume fraction of ethanol 65%, ultrasonic power 500W, investigate the pH value and in 2,4,6,8,10 scopes, the pea total flavones is extracted the impact of yield, finally determine under the pH=8 condition, to extract yield the highest.
C: extraction time is on extracting the impact of yield
Be under the condition of 500W at liquid ratio 20: 1,80 ℃ of temperature, volume fraction of ethanol 65%, ultrasonic power, investigate extraction time in, the impact of the pea total flavones being extracted yield in 20min, 30min, 40min, 50min, the 60min scope, the result shows that to extract yield under the 30min condition the highest.
D: ultrasonic power is on extracting the impact of yield
Under the condition of liquid ratio 20: 1, extraction temperature 60 C, extraction time 30min, volume fraction of ethanol 65%, investigate ultrasonic power extracts yield on the pea total flavones in 200W, 300W, 400W, 500W, 600W scope impact, finally determine under the ultrasonic power of 500W, to extract yield the highest.
E: liquid ratio is on extracting the impact of yield
Be under the 500W condition extracting temperature 60 C, extraction time 30min, volume fraction of ethanol 65%, ultrasonic power, investigate liquid ratio is extracted yield to the persimmon leaf in 10: 1,20: 1,30: 1,40: 1,50: 1 scopes impact, the result shows that to extract gained extraction yield with 20: 1 liquid ratio the highest.
F: extract temperature to extracting the impact of yield
Be under the condition of 500W at liquid ratio 20: 1, time 30min, volume fraction of ethanol 65%, ultrasonic power, investigate and extract temperature is extracted yield on the pea total flavones in 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃ scopes impact, the result shows that the extraction yield is the highest under 60 ℃ of conditions.
3, the response curved surface is optimized extraction conditions
Adopting Response Surface Method research extraction temperature range is 50 ℃, and 60 ℃, 70 ℃, liquid ratio scope are 10: 1, and 20: 1,30: 1, volume fraction of ethanol scope were 50%, 65%, 80%.Other conditions are ultrasonic power 500W, extraction time 30min, pH=8.By the response surface experimental design, the optimised process that final definite ultrasonic Assisted Ethanol extracts the pea total flavones is: 60.86 ℃ of temperature, volume fraction of ethanol 63.58%, liquid ratio 20.80: 1 (mL/g), this moment, the yield of pea total flavones reached 2.100mg/g.
Claims (1)
1. the method for an extracting general flavone from peas in ultrasound-assisted way is characterized in that, comprises the steps:
(1) processing of bean powder
Pea is dried to water ratio≤5%, put into medicinal herb grinder and pulverize, sieve; Bean powder after sieving refluxes with sherwood oil and removes lipid and pigment, and the bean powder after then will refluxing is dried the bean powder that must handle well to water ratio≤3% as for thermostatic drying chamber;
(2) extract
The bean powder that step (1) is handled well is that 20.80:1 mixes with ethanolic soln by liquid ratio, volume grade of alcohol is 63.85% in the ethanolic soln, it is 60.86 ℃ in temperature, ultrasonic power is 500W, the pH value is that 8 condition supersound extraction obtained the total flavones extracting solution in 30 minutes, extracting solution obtains general flavone ethanol-aqueous solution through centrifugal 10 minutes of 10000r/min suction filtration then; General flavone ethanol-aqueous solution is removed ethanol through rotary evaporation, then obtains the total flavones powder with the vacuum freeze drier drying.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104402854A (en) * | 2014-11-12 | 2015-03-11 | 重庆市畜牧科学院 | Method for extracting quercetin from mulberry leaves by utilizing ultrasonic waves |
| CN105748570A (en) * | 2016-04-29 | 2016-07-13 | 中国农业科学院北京畜牧兽医研究所 | Ultrasonic-assisted method for extracting total flavonoid in alfalfa |
| CN105963336A (en) * | 2016-05-11 | 2016-09-28 | 卢鑫 | Extraction method of persimmon leaf total flavonoids |
| CN109022122A (en) * | 2018-07-12 | 2018-12-18 | 广西西林县农本生物科技有限公司 | The method of ultrasound assisted extraction ginger oil |
| CN111388373A (en) * | 2020-04-10 | 2020-07-10 | 蚌埠天泽家用化学品有限公司 | Water-locking moisturizing night cream suitable for dry skin |
| CN115844938B (en) * | 2022-11-29 | 2024-01-26 | 内蒙古农业大学 | Artemisia sphaerocephala total flavone and preparation method and application thereof |
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| CN1395573A (en) * | 2000-01-11 | 2003-02-05 | 比奥雷克斯健康有限公司 | Extraction of flavonoids |
| CN1830464A (en) * | 2005-03-07 | 2006-09-13 | 骏神生物医学（上海）有限公司 | Application of olecranone bean extraction in preparation of food for preventing and treating obesity and type II diabetes |
| CN101391016A (en) * | 2008-10-31 | 2009-03-25 | 山东省农业科学院土壤肥料研究所 | Extraction technique of burdock, soja or garlic extract |
| CN101686704A (en) * | 2007-07-03 | 2010-03-31 | 索莱有限责任公司 | Modified vegetable protein having low levels of phytic acid, isoflavones and ash |
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Patent Citations (4)
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| CN1395573A (en) * | 2000-01-11 | 2003-02-05 | 比奥雷克斯健康有限公司 | Extraction of flavonoids |
| CN1830464A (en) * | 2005-03-07 | 2006-09-13 | 骏神生物医学（上海）有限公司 | Application of olecranone bean extraction in preparation of food for preventing and treating obesity and type II diabetes |
| CN101686704A (en) * | 2007-07-03 | 2010-03-31 | 索莱有限责任公司 | Modified vegetable protein having low levels of phytic acid, isoflavones and ash |
| CN101391016A (en) * | 2008-10-31 | 2009-03-25 | 山东省农业科学院土壤肥料研究所 | Extraction technique of burdock, soja or garlic extract |
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