CN103585424A - Method for extracting total flavone from Chinese chive seeds - Google Patents
Method for extracting total flavone from Chinese chive seeds Download PDFInfo
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- CN103585424A CN103585424A CN201310594282.8A CN201310594282A CN103585424A CN 103585424 A CN103585424 A CN 103585424A CN 201310594282 A CN201310594282 A CN 201310594282A CN 103585424 A CN103585424 A CN 103585424A
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Abstract
The invention relates to a method for extracting total flavone from Chinese chive seeds. The method comprises the following steps: drying and smashing Chinese chive seeds, placing the dried and smashed Chinese chive seeds into an ethanol solution with the mass concentration of 40-99% for soaking for 1-3 hours, and then performing supersonic extraction, so as to obtain an extracting solution, wherein the material-liquid ratio of the Chinese chive seeds to ethanol is (1:10)-(1:50); performing suction filtration on the extracting solution by using qualitative filter paper, further filtering by using a millipore filter after the suction filtration, then concentrating the filter liquor to 10-80% of the original volume of the filter liquor; enabling the concentrated filter liquor to flow through an AB-8 type macroporous adsorptive resin column to be adsorbed for 1-3 hours, washing the AB-8 type macroporous adsorptive resin column adsorbing the filter liquor by using water, and then performing alcohol washing on the washed AB-8 type macroporous adsorptive resin column by using an ethanol solution with the mass concentration of 30-95%; pouring eluant obtained after the alcohol washing into a freezer dryer to be frozen and dried, so that the Chinese chive seed total flavone can be obtained after drying. Compared with the prior art, the method is simple in process, low in cost, and high in extracted total flavone purity, and provides a basis for the development of health care and medical value of the Chinese chive seeds.
Description
Technical field
The present invention relates to a kind of total flavone extracting method, especially relate to a kind of method of extracting total flavones from leek seed.
Background technology
Leek seed is abundant in China's output, and it is the seed of the drying and ripening of edible vegetable liliaceous plant Folium Allii tuberosi, and leek seed (being often called " Semen Allii Tuberosi " in pharmacopeia) is China's Chinese medicine kind.According to pharmacopeia, record, leek seed has the effect of " temperature compensation Liver and kidney, tonifying YANG controlling nocturnal emission with astringent drugs ", Semen Allii Tuberosi as a kind of strengthening yang and invigorating kidney medication in China's history of existing thousands of years among the people.In prior art, have by leek seed the report for the preparation of health foods such as strengthening yang and invigorating kidney, defying age, resisting fatigue, Cardiovarsculars, but from leek seed, extract prepare total flavones research seldom, in research leek seed, total flavones extracts, significant to making full use of the leek seed resource of China's abundant, for health care and the medical value exploitation of leek seed provides experimental basis.
Two of flavone compound general references have a series of compounds that the phenyl ring (A-and B-encircle) of phenolic hydroxyl group links mutually by central thricarbon atom, and its basic parent nucleus is 2-phenyl chromone.Flavone is rich content in natural certain plants and berry, and the nearly kind more than 4,000 of sum, comprises rutin, hesperidin, quercimentin, green tea polyphenol, pattern glucosides, pattern thuja acid etc.The effect of flavone is many-sided, and it is a kind of very strong antioxidant, can effectively remove the oxygen-derived free radicals in body.Flavone can improve blood circulation, reduces cholesterol, treatment cardiovascular and cerebrovascular disease.In addition, flavone also has the effects such as anticancer, enhancing human body immunity power.
Ultrasound assisted extraction technique is by a series of physics and chemistry effect, thereby accelerate effective ingredient, enters solvent, promotes the carrying out of extracting.Ultrasonic extraction has short, the advantage such as productive rate is high, mild condition of extraction time.Alcohol steep and ultrasonic assisted Extraction are followed the example of the total flavones that can obtain high yield, and this method has the features such as pollution-free, environmentally friendly.
The people such as Wu Limei adopt the mode of supercritical carbon dioxide extraction to carry out removing oil in the extraction of < < different cultivars leek seed flavone and antioxidant activity research > > mono-literary composition thereof, and then residue is used for extracting flavone.Because the enforcement of supercritical carbon dioxide extraction needs condition comparatively strict, do not there is general applicability.
Summary of the invention
Object of the present invention is exactly to provide in order to overcome the defect of above-mentioned prior art existence a kind of method of extracting total flavones from leek seed that technique is simple, production cost is low, product purity is high.
Object of the present invention can be achieved through the following technical solutions:
A method of extracting total flavones from leek seed, comprises the following steps:
(1) after leek seed dry is pulverized, put into mass concentration and be alcohol solution dipping 1～3h of 40～99%, the solid-liquid ratio of leek seed and ethanol is 1:10～1:50, and then supersound extraction, obtains extracting solution;
(2) extracting solution is carried out to sucking filtration with qualitative filter paper, after sucking filtration, with microporous filter membrane, further filter, then by 10～80% of filtrate simmer down to filtrate original volume:
(3) filtrate flow after concentrated is adsorbed to 1～3h through AB-8 type macroporous adsorptive resins, water is washed the AB-8 type macroporous adsorptive resins of absorption filtrate, and the alcoholic solution that is then 30%～95% by mass concentration carries out alcohol wash to the AB-8 type macroporous adsorptive resins of washing;
(4) eluent obtaining after alcohol wash is put into freezer dryer and carry out lyophilization, after being dried, obtain leek seed total flavone.
In step (1), the bake out temperature of leek seed is 90～110 ℃, and the drying time of leek seed is 2～5 hours.
In step (1), leek seed obtains 50～100 object leek seed powder after pulverizing.
In step (1), the temperature of supersound extraction is 20～60 ℃, and the time of supersound extraction is 10～60min.
As preferably, in step (1), the temperature of supersound extraction is 30～50 ℃.
In step (3), to the time that the AB-8 type macroporous adsorptive resins of absorption filtrate is washed be 35～55min, the time of the AB-8 type macroporous adsorptive resins of washing being carried out to alcohol wash is 1～3h.
In step (4), cryodesiccated temperature is-20 ℃～50 ℃, and the cryodesiccated time is 2～5h.
In step (4), under the environment that lyophilization is is 1～10Pa in vacuum, carry out.
Compared with prior art, technique of the present invention is simple, and cost is low, and the total flavones purity of extraction is high, by the health care for leek seed and medical value exploitation, provides foundation.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
Leek seed is dried to 5h in temperature is the drying baker of 90 ℃, pulverize and sieve, obtain 70～100 object granules, put into mass concentration and be 60% alcoholic solution lixiviate 2h, 30 ℃ of temperature, solid-liquid ratio is 1:10, supersound extraction 1h;
Extracting solution is carried out to sucking filtration with qualitative filter paper, then by 50% of filtrate simmer down to original volume;
Filtrate flow after concentrated is adsorbed to 2h through AB-8 type macroporous adsorptive resins, water is washed 40min to the AB-8 type macroporous adsorptive resins of absorption filtrate, and the alcoholic solution that is then 50% by mass concentration carries out alcohol wash 1h to AB-8 type macroporous adsorptive resins;
Then the freezer dryer of the eluent of alcohol wash being put into vacuum and be 1Pa is dried, and the time is 5h, and temperature is-20 ℃, obtains leek seed total flavone after dry.
Productive rate 2.6 ‰, purity is greater than 90%.
Embodiment 2
Leek seed is dried to 2h in temperature is the drying baker of 110 ℃, pulverize and sieve, obtain 50～100 object granules, put into mass concentration and be 70% alcoholic solution lixiviate 2h, temperature 50 C, solid-liquid ratio is 1:50, supersound extraction 1h;
Extracting solution is carried out to sucking filtration with qualitative filter paper, then by 50% of filtrate simmer down to original volume;
Filtrate flow after concentrated is adsorbed to 2h through AB-8 type macroporous adsorptive resins, water is washed 40min to the AB-8 type macroporous adsorptive resins of absorption filtrate, and the alcoholic solution that is then 30% by mass concentration carries out alcohol wash 1h to AB-8 type macroporous adsorptive resins;
Then the freezer dryer of the eluent of alcohol wash being put into vacuum and be 10Pa is dried, and the time is 2h, and temperature is-50 ℃, obtains leek seed total flavone after dry.
Productive rate 3 ‰, purity is greater than 90%.
Embodiment 3
Leek seed is dried to 3h in temperature is the drying baker of 100 ℃, pulverize and sieve, obtain 70～100 object granules, put into mass concentration and be 40% alcoholic solution lixiviate 3h, 20 ℃ of temperature, solid-liquid ratio is 1:20, supersound extraction 1h;
Extracting solution is carried out to sucking filtration with qualitative filter paper, then by 80% of filtrate simmer down to original volume;
Filtrate flow after concentrated is adsorbed to 3h through AB-8 type macroporous adsorptive resins, water is washed 55min to the AB-8 type macroporous adsorptive resins of absorption filtrate, and the alcoholic solution that is then 50% by mass concentration carries out alcohol wash 3h to AB-8 type macroporous adsorptive resins;
Then the freezer dryer of the eluent of alcohol wash being put into vacuum and be 5Pa is dried, and the time is 3h, and temperature is-30 ℃, obtains leek seed total flavone after dry.
Productive rate 2.8 ‰, purity is greater than 90%.
Embodiment 4
Leek seed is dried to 4h in temperature is the drying baker of 100 ℃, pulverize and sieve, obtain 70～100 object granules, put into mass concentration and be 99% alcoholic solution water-bath and extract 1h, 60 ℃, solid-liquid ratio is 1:30, supersound extraction 10min;
Extracting solution is carried out to sucking filtration with qualitative filter paper, then by 10% of filtrate simmer down to original volume;
Filtrate flow after concentrated is adsorbed to 1h through AB-8 type macroporous adsorptive resins, water is washed 35min to the AB-8 type macroporous adsorptive resins of absorption filtrate, and the alcoholic solution that is then 95% by mass concentration carries out alcohol wash 1h to AB-8 type macroporous adsorptive resins;
Then the freezer dryer of the eluent of alcohol wash being put into vacuum and be 8Pa is dried, and the time is 4h, and temperature is-25 ℃, obtains leek seed total flavone after dry.
Productive rate 3.1 ‰, purity is greater than 90%.
Embodiment 5
Leek seed is dried to 5h in temperature is the drying baker of 90 ℃, pulverize and sieve, obtain 50～100 object granules, put into mass concentration and be 70% alcoholic solution water-bath and extract 3h, 40 ℃ of temperature, solid-liquid ratio is 1:20, supersound extraction 0.5h;
Extracting solution is carried out to sucking filtration with qualitative filter paper, then by 30% of filtrate simmer down to original volume;
Filtrate flow after concentrated is adsorbed to 2h through AB-8 type macroporous adsorptive resins, water is washed 40min to the AB-8 type macroporous adsorptive resins of absorption filtrate, and the alcoholic solution that is then 50% by mass concentration carries out alcohol wash 2h to AB-8 type macroporous adsorptive resins;
Then the freezer dryer of the eluent of alcohol wash being put into vacuum and be 3Pa is dried, and the time is 4h, and temperature is-40 ℃, obtains leek seed total flavone after dry.
Productive rate 3.1 ‰, purity is greater than 90%.
Embodiment 6
Leek seed is dried to 3h in temperature is the drying baker of 95 ℃, pulverize and sieve, obtain 50～100 object granules, put into mass concentration and be 50% alcoholic solution lixiviate 2h, 45 ℃, solid-liquid ratio is 1:30, supersound extraction 40min;
Extracting solution is carried out to sucking filtration with qualitative filter paper, then by 65% of filtrate simmer down to original volume;
Filtrate flow after concentrated is adsorbed to 2h through AB-8 type macroporous adsorptive resins, water is washed 45min to the AB-8 type macroporous adsorptive resins of absorption filtrate, and the alcoholic solution that is then 40% by mass concentration carries out alcohol wash 2h to AB-8 type macroporous adsorptive resins;
Then the freezer dryer of the eluent of alcohol wash being put into vacuum and be 3Pa is dried, and the time is 4h, and temperature is-40 ℃, obtains leek seed total flavone after dry.
Productive rate 3.2 ‰, purity is greater than 90%.
Above-described embodiment is interpreted as only for the present invention is described, is not used in and limits the scope of the invention.After having read the content of the present invention's record, those skilled in the art can make various changes or modifications the present invention, and these equivalences change and modification falls into the scope of the claims in the present invention equally.
Claims (8)
1. from leek seed, extract a method for total flavones, it is characterized in that, comprise the following steps:
(1) after leek seed dry is pulverized, put into mass concentration and be alcohol solution dipping 1～3h of 40～99%, the solid-liquid ratio of leek seed and ethanol is 1:10～1:50, and then supersound extraction, obtains extracting solution;
(2) extracting solution is carried out to sucking filtration with qualitative filter paper, after sucking filtration, with microporous filter membrane, further filter, then by 10～80% of filtrate simmer down to filtrate original volume;
(3) filtrate flow after concentrated is adsorbed to 1～3h through AB-8 type macroporous adsorptive resins, water is washed the AB-8 type macroporous adsorptive resins of absorption filtrate, and the alcoholic solution that is then 30%～95% by mass concentration carries out alcohol wash to the AB-8 type macroporous adsorptive resins of washing;
(4) eluent obtaining after alcohol wash is put into freezer dryer and carry out lyophilization, after being dried, obtain leek seed total flavone.
2. a kind of method of extracting total flavones from leek seed according to claim 1, is characterized in that, in step (1), the bake out temperature of leek seed is 90～110 ℃, and the drying time of leek seed is 2～5 hours.
3. a kind of method of extracting total flavones from leek seed according to claim 1, is characterized in that, in step (1), leek seed obtains 50～100 object leek seed powder after pulverizing.
4. a kind of method of extracting total flavones from leek seed according to claim 1, is characterized in that, in step (1), the temperature of supersound extraction is 20～60 ℃, and the time of supersound extraction is 10～60min.
5. a kind of method of extracting total flavones from leek seed according to claim 4, is characterized in that, in step (1), the temperature of supersound extraction is 30～50 ℃.
6. a kind of method of extracting total flavones from leek seed according to claim 1, it is characterized in that, in step (3), to the time that the AB-8 type macroporous adsorptive resins of absorption filtrate is washed be 35～55min, the time of the AB-8 type macroporous adsorptive resins of washing being carried out to alcohol wash is 1～3h.
7. a kind of method of extracting total flavones from leek seed according to claim 1, is characterized in that, in step (4), cryodesiccated temperature is-20 ℃～-50 ℃, and the cryodesiccated time is 2～5h.
8. a kind of method of extracting total flavones from leek seed according to claim 1, is characterized in that, in step (4), under the environment that lyophilization is is 1～10Pa in vacuum, carries out.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104983776A (en) * | 2014-08-10 | 2015-10-21 | 胡刘满 | Energy-saving equipment for extracting rhododendron general flavone |
| CN111658724A (en) * | 2020-05-21 | 2020-09-15 | 安徽金龙源生物科技有限公司 | Preparation method and application of leek seed extract |
| CN114365853A (en) * | 2022-02-15 | 2022-04-19 | 江西师范大学 | Method for preparing antioxidant dietary fiber in citrus peel residues |
| WO2023065264A1 (en) * | 2021-10-22 | 2023-04-27 | 南通优元美术图案设计有限公司 | Enrichment tube for enriching total flavonoids in chinese chives seed extraction solution |
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Non-Patent Citations (2)
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| 武丽梅等: "不同品种韭菜籽黄酮提取及其抗氧化活性研究", 《上海市化学化工学会2011年度学术年会论文集》, 1 November 2011 (2011-11-01), pages 26 - 28 * |
| 葛淑兰等: "大孔吸附树脂及其在黄酮类成分分离纯化中的应用进展", 《中国药师》, vol. 11, no. 6, 31 December 2008 (2008-12-31), pages 702 - 705 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104983776A (en) * | 2014-08-10 | 2015-10-21 | 胡刘满 | Energy-saving equipment for extracting rhododendron general flavone |
| CN104983776B (en) * | 2014-08-10 | 2020-12-15 | 苏州果汁网信息科技有限公司 | Energy-saving equipment for extracting total flavonoids of rhododendron simsii |
| CN111658724A (en) * | 2020-05-21 | 2020-09-15 | 安徽金龙源生物科技有限公司 | Preparation method and application of leek seed extract |
| WO2023065264A1 (en) * | 2021-10-22 | 2023-04-27 | 南通优元美术图案设计有限公司 | Enrichment tube for enriching total flavonoids in chinese chives seed extraction solution |
| CN114365853A (en) * | 2022-02-15 | 2022-04-19 | 江西师范大学 | Method for preparing antioxidant dietary fiber in citrus peel residues |
| CN114365853B (en) * | 2022-02-15 | 2023-11-10 | 江西师范大学 | Method for preparing antioxidant dietary fibers in citrus peel residues |
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