CN101879208A - Method for extracting total flavonoids from mung bean shell - Google Patents
Method for extracting total flavonoids from mung bean shell Download PDFInfo
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- CN101879208A CN101879208A CN2010101568288A CN201010156828A CN101879208A CN 101879208 A CN101879208 A CN 101879208A CN 2010101568288 A CN2010101568288 A CN 2010101568288A CN 201010156828 A CN201010156828 A CN 201010156828A CN 101879208 A CN101879208 A CN 101879208A
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Abstract
The invention relates to a method for extracting total flavonoids from a mung bean shell, which comprises the following steps: taking the mung bean shell as a raw material, carrying out microwave extraction twice to three times with 30-50 percent of ethanol, adsorbing twice to three times with an acidity-adjusting rapid upper column, eluting flavonoids with ethanol, carrying out concentrative crystallization, removing impurities in a method of alkali-extraction and acid-precipitation, and recrystallizing with 90-99 percent of ethanol. The product prepared with the process has the advantages of high content and high quality, and can be used as the additive for health care products and food.
Description
Technical field:
The present invention relates to a kind of method of from mung bean shell, extracting total flavones, the method that total flavones is produced in especially a kind of microwave extraction, the absorption of acid adjustment rapid resin.
Background technology:
Semen phaseoli radiati (Mung bean) has another name called Semen phaseoli radiati, and the record bean is planted bean, is the mature seed of leguminous herbaceous plant's Semen phaseoli radiati, is medicine food dual purpose plant.The traditional Chinese medical science thinks that it is sweet in flavor and cold in property, and refreshing and detoxicating is arranged, antidiarrheal diuresis, the detumescence therapeutic method to keep the adverse QI flowing downwards, the effect of heat clearing away and restlessness relieving and nourishing and fit keeping function.
As the garbage Testa Phaseoli radiati of food, the traditional Chinese medical science is referred to as mung bean shell or testa mungo.It contains flavone, tannin, and Saponin, alkaloid, cardiotonic glycoside, the chemical constituent of biologically actives such as anthraquinone analog compound, drug action is better than other parts of Semen phaseoli radiati.Wherein flavones ingredient has antioxidation, enhancing immunity, and effects such as blood fat reducing, blood glucose become the focus of health product in recent years.
The method of extracting flavone both at home and abroad is a lot, and water-boiling method, organic solvent extraction method, enzymatic isolation method, supercritical extraction, ultrasonic extraction, microwave extraction method are arranged.The method of separating flavone has resin adsorption method, high performance liquid chromatography etc.Extract the flavone method from Testa Phaseoli radiati, be generally the research of extraction ratio, the document disclosed methods such as " optimization of Flavonoid substances extracting condition are studied in the Testa Phaseoli radiati " that " extracting the research of flavone technology in the mung bean shell " of delivering as Zhang Yanjie etc. and Su Bingxia etc. deliver is the optimization technology of the extraction conditions of Semen phaseoli radiati flavone.The disclosed method of number of patent application 200910172923 " extracting method of flavone compound in the Testa Phaseoli radiati " is to adopt extruding puffing, and ethanol extraction also just improves the method for extraction ratio.From mung bean shell, extract the method for high-load total flavones, open very few.
Summary of the invention:
The technical problem to be solved in the present invention provides a kind of method of extracting total flavones from mung bean shell.This method can access high-load total flavones, and with short production cycle, is convenient to the industrialization operation.
Extractive technique scheme of the present invention is as follows:
A kind of method of from mung bean shell, extracting total flavones, it is characterized in that comprising following steps: with the coarse pulverization of mung bean shell raw material, add 6-20 and doubly measured 30-50% alcohol solution dipping microwave 1-2 hour, extract 2-3 time, merge extractive liquid, adds 0.3-1% (v/v) mineral acid, fast by macroporous resin column absorption 2-3 time, water alcohol gradient elution, the eluent concentrating under reduced pressure that contains the flavone flow point does not have pure crystallization, leach to such an extent that total flavones crude product aqueous alkali dissolves the acid adjustment precipitating 2-3 time, the precipitating thing is 90%-99% alcohol reflux dissolving-recrystallization 1-2 time again, and drying promptly gets product.
Described microwave extracting power 1-20KW.
Described macroporous resin is polar macroporous resin.Preferred NKA-9, ADS-21 or ADS-7.
Described upper prop absorption flow velocity is 8-15BVh
-1Flow velocity passes through resin column.
Described water alcohol gradient elution is: wash neutrality 4-6BV60-90% ethanol elution flavone more earlier.Preferred 70% ethanol elution.
The molten acid adjustment precipitating of described alkali condition is: aqueous alkali is the inorganic strong alkali aqueous solution of pH 10-12, and acid is inorganic acid.Transferring to ph4-5 is advisable.
In sum, there is following advantage in the present invention:
1) microwave-assisted extracts, and mung bean shell is difficult for gelatinizing, the extraction efficiency height.
2) utilize adjusting solvent pH, can improve flavone can be beneficial to purification by resin absorption character in low alcohol, and the mother solution after the absorption need not to reclaim can do extraction solution, energy savings again.
3) upward column flow rate is fast, and repeatedly upper prop absorption absorption is thorough, and the cycle is short.
4) whole operation does not have the toxic reagent use, and the products obtained therefrom purity quality is good, can cook health product and food additive.
Further specify the present invention below in conjunction with the specific embodiment, but the scope of protection of present invention is not limited to following embodiment.
The specific embodiment:
Embodiment 1:
The mung bean shell coarse pulverization, get 1kg and 6L30% ethanol and drop into microwave extraction tank, open power 2KW and extracted 1 hour, extracts 3 times, filtration merge extracting solution 17L, add the 170ml mixed in hydrochloric acid, get 700ml and handled macroporous resin NKA-9 dress post, extracting solution is added resin column, flow speed control 5.6ml/h, adsorb 2 times, lower column liquid is transferred pH neutrality to do extracting solution and is used.Remove ionized water eluting resin column to neutral, get 4.2L60% ethanol elution total flavones again, collect flavone flow point concentrating under reduced pressure and do not have alcohol, place crystallization.Leach crystal and get 24g, after the sodium hydrate aqueous solution dissolving with ph10, hydrochloric acid is regulated neutral precipitating, repeats 3 times, and the precipitating thing leaches with the dissolving of 90% alcohol reflux and leaves standstill crystallization, leaches exsiccant total flavones 12g, content 90%.
Embodiment 2:
The mung bean shell coarse pulverization, get 1kg and 6L40% ethanol and drop into microwave extraction tank, open power 2KW and extracted 1 hour, extracts 3 times, filtration merge extracting solution 18L, adding 80ml sulphuric acid mixes, get 700ml and handled macroporous resin ADS-21 dress post, extracting solution is added resin column, flow speed control 10ml/h, adsorb 3 times, lower column liquid is transferred pH neutrality to do extracting solution and is used.Remove ionized water eluting resin column to neutral, get 3L90% ethanol elution total flavones again, collect flavone flow point concentrating under reduced pressure and do not have alcohol, place crystallization.Leach crystal and get 28g, after the sodium hydrate aqueous solution dissolving with ph12, hydrochloric acid is regulated neutral precipitating, repeats 2 times, and the precipitating thing leaches with the dissolving of 90% alcohol reflux and leaves standstill crystallization 2 times, leaches exsiccant total flavones 10g, content 92%.
Embodiment 3:
The mung bean shell coarse pulverization, get 1kg and 6L50% ethanol and drop into microwave extraction tank, open power 2KW and extracted 1 hour, extracts 3 times, filtration merge extracting solution 16L, add the 150ml mixed in hydrochloric acid, get 700ml and handled macroporous resin ADS-7 dress post, extracting solution is added resin column, flow speed control 8ml/h, adsorb 3 times, lower column liquid is transferred pH neutrality to do extracting solution and is used.Remove ionized water eluting resin column to neutral, get 3.5L75% ethanol elution total flavones again, collect flavone flow point concentrating under reduced pressure and do not have alcohol, place crystallization.Leach crystal and get 26g, after the potassium hydroxide aqueous solution dissolving with ph11, sulphuric acid is regulated neutral precipitating, repeats 3 times, and the precipitating thing leaches with the dissolving of 99% alcohol reflux and leaves standstill crystallization, leaches exsiccant total flavones 13g, content 91%.
Embodiment 4:
The mung bean shell coarse pulverization, get 1kg and 8L30% ethanol and drop into microwave extraction tank, open power 1KW and extracted 2 hours, extracts 2 times, filtration merge extracting solution 15L, adding 75ml sulphuric acid mixes, get 700ml and handled macroporous resin ADS-7 dress post, extracting solution is added resin column, flow speed control 10ml/h, adsorb 3 times, lower column liquid is transferred pH neutrality to do extracting solution and is used.Remove ionized water eluting resin column to neutral, get 3.5L75% ethanol elution total flavones again, collect flavone flow point concentrating under reduced pressure and do not have alcohol, place crystallization.Leach crystal and get 27g, after the potassium hydroxide aqueous solution dissolving with ph10, sulphuric acid is regulated neutral precipitating, repeats 3 times, and the precipitating thing leaches with the dissolving of 90% alcohol reflux and leaves standstill crystallization, leaches exsiccant total flavones 12g, content 90%.
Embodiment 5:
The mung bean shell coarse pulverization, get 5kg and 30L30% ethanol and drop into microwave extraction tank, open power 10KW and extracted 1 hour, extracts 3 times, filtration merge extracting solution 83L, add the 420ml mixed in hydrochloric acid, get 3.5L and handled macroporous resin NKA-9 dress post, extracting solution is added resin column, flow speed control 10ml/h, adsorb 23 times, lower column liquid is transferred pH neutrality to do extracting solution and is used.Remove ionized water eluting resin column to neutral, get 4.2L60% ethanol elution total flavones again, collect flavone flow point concentrating under reduced pressure and do not have alcohol, place crystallization.Leach crystal and get 130g, after the sodium hydrate aqueous solution dissolving with ph10, hydrochloric acid is regulated neutral precipitating, repeats 3 times, and the precipitating thing leaches with the dissolving of 90% alcohol reflux and leaves standstill crystallization, leaches exsiccant total flavones 65g, content 90%.
Claims (6)
1. method of from mung bean shell, extracting total flavones, it is characterized in that comprising following steps: with the coarse pulverization of mung bean shell raw material, add 6-20 and doubly measured 30-50% alcoholic solution microwave extraction 1-2 hour, extract 2-3 time, merge extractive liquid, adds 0.3-1% (v/v) mineral acid, by macroporous resin column absorption 2-3 time, water alcohol gradient elution, the eluent concentrating under reduced pressure that contains the flavone flow point does not have pure crystallization, leach to such an extent that total flavones crude product aqueous alkali dissolves the acid adjustment precipitating 2-3 time, the precipitating thing is 90%-99% alcohol reflux dissolving-recrystallization 1-2 time again, and drying promptly gets product.
2. the method for extracting total flavones from mung bean shell as claimed in claim 1 is characterized in that described microwave extracting power 1-20KW.
3. the method for extracting total flavones from mung bean shell as claimed in claim 1 is characterized in that described macroporous resin is polar macroporous resin.
4. the method for extracting total flavones from mung bean shell as claimed in claim 1 is characterized in that described upper prop absorption flow velocity can be 8-15BVh
-1Flow velocity passes through resin column.
5. the method for extracting total flavones from mung bean shell as claimed in claim 1 is characterized in that described water alcohol gradient elution is: wash neutrality 4-6BV60-90% ethanol elution flavone more earlier.
6. the method for extracting total flavones from mung bean shell as claimed in claim 1, it is characterized in that the molten acid adjustment precipitating of described alkali condition is: aqueous alkali is the inorganic strong alkali aqueous solution of pH10-12, and acid is inorganic acid.
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| CN2010101568288A CN101879208A (en) | 2010-04-27 | 2010-04-27 | Method for extracting total flavonoids from mung bean shell |
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| CN2010101568288A CN101879208A (en) | 2010-04-27 | 2010-04-27 | Method for extracting total flavonoids from mung bean shell |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105248918A (en) * | 2015-11-25 | 2016-01-20 | 广西职业技术学院 | Pig feed additive |
| 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 |
| CN109512751A (en) * | 2017-09-19 | 2019-03-26 | 赵志坚 | A kind of toothpaste and preparation method thereof containing Semen phaseoli radiati extract |
| WO2019227382A1 (en) * | 2018-05-31 | 2019-12-05 | 京冠生物科技股份有限公司 | Mung bean hull extract with antiviral effect and extraction method therefor |
-
2010
- 2010-04-27 CN CN2010101568288A patent/CN101879208A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105248918A (en) * | 2015-11-25 | 2016-01-20 | 广西职业技术学院 | Pig feed additive |
| 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 |
| CN109512751A (en) * | 2017-09-19 | 2019-03-26 | 赵志坚 | A kind of toothpaste and preparation method thereof containing Semen phaseoli radiati extract |
| WO2019227382A1 (en) * | 2018-05-31 | 2019-12-05 | 京冠生物科技股份有限公司 | Mung bean hull extract with antiviral effect and extraction method therefor |
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Application publication date: 20101110 |