CN102172364A - 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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- CN102172364A CN102172364A CN 201110053244 CN201110053244A CN102172364A CN 102172364 A CN102172364 A CN 102172364A CN 201110053244 CN201110053244 CN 201110053244 CN 201110053244 A CN201110053244 A CN 201110053244A CN 102172364 A CN102172364 A CN 102172364A
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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 Semen Pisi sativi total flavones, the method for total flavones in especially a kind of ultrasonic assisted extraction Semen Pisi sativi.
Background technology
The extraction of Semen Pisi sativi total flavones method commonly used is a solvent extraction method at present, and solvent extraction method comprises hot water extraction method and organic solvent extraction method.The hot water extraction method only can be used for extracting strong polar chromocor compound, and it is low to extract yield, and extraction time is long, solvent consumption is big; Impurity such as the protein saccharide 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 big; The product residue organic solvent that extracts is unfavorable for the food service industry application; The Enzymatic Extraction selectivity is better, but the cost height, and yield is lower.
In addition: extract method for designing at present and mainly concentrate on and carry out orthogonal optimization, though it has a lot of superioritys than experiment of single factor commonly used, experiment number obviously reduces; Can obtain secondary factors that influences experimental result etc. by variance analysis.But, make that orthogonal method is not that total energy obtains best optimal conditions owing to often have reciprocal action between factor.Orthogonal Optimization can only be handled discrete horizontal factor, obtain that prioritization scheme then need 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 reciprocal action thereof, can do regression analysis to concentrating factor interaction, the optimization data that obtain are more approaching effectively more near true horizon, thereby more with practical value.The influence that the 3-D graphic that response surface analysis obtains can very intuitively must be found out each factor to experimental result.
Summary of the invention
Technical problem to be solved by this invention is to provide at the existing problem of the solvent extraction method of above-mentioned Semen Pisi sativi total flavones the method for total flavones in a kind of ultrasonic assisted extraction Semen Pisi sativi, this 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, do not have chemical reaction therebetween, reduced the change of bioactive substance.
Technical problem to be solved by this invention can be achieved through the following technical solutions:
The method of total flavones comprises the steps: in a kind of ultrasonic assisted extraction Semen Pisi sativi
(1) processing of Semen Glycines powder
Semen Pisi sativi is dried to moisture content≤5%, put into Chinese medicine grinder and pulverize, sieve; Semen Glycines powder after sieving refluxes with petroleum ether and removes lipid and pigment, and the Semen Glycines powder after will refluxing is then dried the Semen Glycines powder that must handle well to moisture content≤3% as for thermostatic drying chamber;
(2) extract
The Semen Glycines powder that step (1) is handled well and alcoholic solution are to mix in 10: 1～50: 1 by liquid material ratio, alcoholic acid volume fraction is 20～80% in the alcoholic solution, in temperature is 50～90 ℃, ultrasonic power is 200～600W, 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 sucking filtration then.General flavone ethanol-aqueous solution is removed ethanol through rotary evaporation, obtains the total flavones powder with the vacuum freeze drier drying then.
In a preferred embodiment of the invention, in the described step (2), alcoholic acid volume fraction is preferably 65% in the alcoholic solution.
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 material 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 the ethanol volume fraction 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, do not have chemical reaction therebetween, reduced the change of bioactive substance.
The specific embodiment
The following examples can help those skilled in the art more fully to understand the present invention, but do not limit the present invention in any way.
The method of total flavones comprises the steps: in a kind of ultrasonic assisted extraction Semen Pisi sativi
1, the preparation of Semen Glycines powder
Semen Pisi sativi in 80 ℃ of thermostatic drying chamber oven dry 3 hours, is put into Chinese medicine grinder and pulverized, and it is standby to cross 80 mesh sieves.Semen Glycines powder after sieving refluxes with petroleum ether and removed lipid and pigment in 2 hours, the Semen Glycines powder that the Semen Glycines powder after will refluxing then must be handled well as for 80 ℃ of oven dry of thermostatic drying chamber in 3 hours.
2, extract
The Semen Glycines powder that step (1) is handled well and alcoholic solution are to mix in 10: 1～50: 1 by liquid material ratio, alcoholic acid volume fraction is 20～80% in the alcoholic solution, in temperature is 50～90 ℃, ultrasonic power is 200～600W, 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 sucking filtration then.General flavone ethanol-aqueous solution is removed ethanol through rotary evaporation, obtains the total flavones powder with the vacuum freeze drier drying then.
Test below by single factor experiment method and the influence that response curved surface optimization extracts yield to ultrasonic power, extraction temperature, extraction time, ethanol volume fraction, the comparison of liquid material, with ultrasonic power, extraction temperature, extraction time, ethanol volume fraction, the liquid material ratio of choosing optimization.
1, single factor experiment comprises: ultrasonic power, the influence of extracting temperature, extraction time, ethanol volume fraction, liquid material comparison extraction 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 the influence that temperature, liquid material ratio, ethanol volume fraction and liquid material comparison Semen Pisi sativi total flavones extract yield.Specific implementation method sees Table 2
Table 2 response surface experimental factor and level
Result of the test:
A: the ethanol volume fraction is to extracting the influence of yield
Is under the condition of 600W at the liquid material than 20: 1,80 ℃ of temperature, time 20min, ultrasonic power, investigate the ethanol volume fraction and the Semen Pisi sativi total flavones is extracted the influence of yield in 20%, 35%, 50%, 65%, 80% scope, the result shows that the ethanol extraction gained extraction yield with 65% is the highest.
The b:pH value is to extracting the influence of yield
The liquid material than 20: 1, extract under the condition of 60 ℃ of temperature, extraction time 30min, ethanol volume fraction 65%, ultrasonic power 500W, investigate pH value extracts yield to the Semen Pisi sativi total flavones in 2,4,6,8,10 scopes influence, it is the highest finally to determine to extract yield under the pH=8 condition.
C: extraction time is to extracting the influence of yield
Is under the condition of 500W at the liquid material than 20: 1,80 ℃ of temperature, ethanol volume fraction 65%, ultrasonic power, investigate extraction time in, the influence of the Semen Pisi sativi 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 to extracting the influence of yield
The liquid material than 20: 1, extract under the condition of 60 ℃ of temperature, extraction time 30min, ethanol volume fraction 65%, investigate ultrasonic power extracts yield to the Semen Pisi sativi total flavones in 200W, 300W, 400W, 500W, 600W scope influence, it is the highest finally to determine to extract yield under the ultrasonic power of 500W.
E: the influence that yield is extracted in the comparison of liquid material
At 60 ℃ of temperature of extraction, extraction time 30min, ethanol volume fraction 65%, ultrasonic power is under the 500W condition, investigate the liquid material than the influence of in 10: 1,20: 1,30: 1,40: 1,50: 1 scopes Folium Kaki being extracted yield, the result shows with 20: 1 liquid material higher than extracting gained extraction yield.
F: extract temperature to extracting the influence of yield
Is under the condition of 500W at the liquid material than 20: 1, time 30min, ethanol volume fraction 65%, ultrasonic power, investigate and extract temperature is extracted yield to the Semen Pisi sativi total flavones in 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃ scopes influence, 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 material are 10: 1 than scope, and 20: 1,30: 1, ethanol volume fraction scope were 50%, 65%, 80%.Other conditions are ultrasonic power 500W, extraction time 30min, pH=8.By the response surface experimental design, determine that finally the optimised process of ultrasonic auxiliary ethanol extraction Semen Pisi sativi total flavones is: 60.86 ℃ of temperature, ethanol volume fraction 63.58%, liquid material were than 20.80: 1 (mL/g), and this moment, the yield of Semen Pisi sativi total flavones reached 2.100mg/g.
Claims (8)
1. the method for total flavones in the ultrasonic assisted extraction Semen Pisi sativi is characterized in that, comprises the steps:
(1) processing of Semen Glycines powder
Semen Pisi sativi is dried to moisture content≤5%, put into Chinese medicine grinder and pulverize, sieve; Semen Glycines powder after sieving refluxes with petroleum ether and removes lipid and pigment, and the Semen Glycines powder after will refluxing is then dried the Semen Glycines powder that must handle well to moisture content≤3% as for thermostatic drying chamber;
(2) extract
The Semen Glycines powder that step (1) is handled well and alcoholic solution are to mix in 10: 1～50: 1 by liquid material ratio, alcoholic acid volume fraction is 20～80% in the alcoholic solution, in temperature is 50～90 ℃, ultrasonic power is 200～600W, 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 sucking filtration then.General flavone ethanol-aqueous solution is removed ethanol through rotary evaporation, obtains the total flavones powder with the vacuum freeze drier drying then.
2. the method for total flavones is characterized in that in a kind of ultrasonic assisted extraction Semen Pisi sativi as claimed in claim 1, and in the described step (2), alcoholic acid volume fraction is 65% in the alcoholic solution.
3. the method for total flavones is characterized in that in a kind of ultrasonic assisted extraction Semen Pisi sativi as claimed in claim 1, and in the described step (2), its pH value is 8.
4. the method for total flavones is characterized in that in a kind of ultrasonic assisted extraction Semen Pisi sativi as claimed in claim 1, and in the described step (2), the supersound extraction time is 30 minutes.
5. the method for total flavones is characterized in that in a kind of ultrasonic assisted extraction Semen Pisi sativi as claimed in claim 1, and in the described step (2), ultrasonic power is 500W.
6. the method for total flavones is characterized in that in a kind of ultrasonic assisted extraction Semen Pisi sativi as claimed in claim 1, and in the described step (2), liquid material ratio is 20: 1.
7. the method for total flavones is characterized in that in a kind of ultrasonic assisted extraction Semen Pisi sativi as claimed in claim 1, and in the described step (2), temperature is 60 ℃.
8. the method for total flavones is characterized in that in a kind of ultrasonic assisted extraction Semen Pisi sativi as claimed in claim 1, and in the described step (2), described solid-liquid ratio is 20.80: 1, and temperature is 60.86 ℃, and the ethanol volume fraction is 63.58%.
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Cited By (6)
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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 |
| CN115844938A (en) * | 2022-11-29 | 2023-03-28 | 内蒙古农业大学 | Artemisia sphaerocephala total flavone and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN115844938A (en) * | 2022-11-29 | 2023-03-28 | 内蒙古农业大学 | Artemisia sphaerocephala total flavone and preparation method and application thereof |
| 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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