CN104189087B - A kind of method extracting total flavonoid functional materials from Folium Mori - Google Patents
A kind of method extracting total flavonoid functional materials from Folium Mori Download PDFInfo
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- CN104189087B CN104189087B CN201410395997.5A CN201410395997A CN104189087B CN 104189087 B CN104189087 B CN 104189087B CN 201410395997 A CN201410395997 A CN 201410395997A CN 104189087 B CN104189087 B CN 104189087B
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Abstract
The present invention provides a kind of method extracting total flavonoid functional materials from Folium Mori, belongs to natural product extraction and separation technology field.Carry out as follows: a. cleans: Folium Mori carry out surface drip washing process, washes the dust on Folium Mori；B. preservation: the Folium Mori after cleaning with step a with lactic acid bacteria mix in proportion, and sealing bag or cement pit sealing anaerobic fermentation preservation；C. extract: with the Folium Mori of water cleaning step b preservation, then hydrochloric acid-deionized water and Folium Mori are mixed in proportion reflux, extract, filter, obtain flavones in mulberry leaves crude extract A；D. refine: flavones in mulberry leaves crude extract A is first passed through the ultrafilter membrane of molecular weight 10000-50000Da, collect permeate；Trapped fluid collected by ultrafilter membrane again through molecular weight 100-500Da, after trapped fluid concentration, spray-dried namely obtains Folium Mori total flavonoids product.The inventive method adopts lactic acid bacteria to preserve Folium Mori and extracts flavone, compares traditional fresh mulberry leaf or dry Folium Mori extract flavone, flavones in mulberry leaves extraction ratio can be greatly improved, can reduce the content of macromole saccharide, protein in product simultaneously, improve product purity.Flavone purification aspect, the inventive method utilizes ultrafiltration membrane technique purification flavones in mulberry leaves, large hole purification on adsorbent resins technique energy-conserving and environment-protective more.
Description
Technical field
The present invention relates to natural product extraction and separation technology field, particularly to a kind of method of Folium Mori lactic acid bacteria preservation high efficiency extraction total flavonoid functional materials.
Background technology
China mulberry of a great variety, has the cultivation of mulberry in southern and northern most area.Folium Mori are the primary products of mulberry, but exploitation application at present is less, mostly as offal treatment, causes resource greatly to waste.Being found by pharmacological research, the flavonoid bioactive substance contained in Folium Mori suffers from the effect of highly significant in prevention and treatment diabetes, hypertension, hyperlipidemia and antiviral, defying age, anti-inflammation etc..If its medicine resource is made full use of, then the benefit of its economy and society is by considerable.
At present, extraction and purification about Folium Mori functional materials has more Patents, as CN101412703A discloses a kind of method coproduction of mulberry tea flavone, polysaccharide and alkaloidal composite extracting technique utilizing ethanol water to cross resin, CN101862372A discloses a kind of method utilizing aqueous alkali heating extraction mistake macroporous resin and produces the technique of flavones in mulberry leaves, and CN1762428 discloses and utilizes supercritical carbon dioxide to extract deoxidation nojirimycin Alkaloid and the method for two kinds of effective ingredient of flavone from Folium Mori.Above patent is that one or more have the extraction of bioactive substance in Folium Mori, and extractant mostly is ethanol, and extraction time is long, and it is relatively costly, flavone purification then mostly adopts macroporous adsorbent resin, although this technique can improve flavone purity, but all consumes bigger to material and the energy.Potass extraction shell-broken effect is not so good as sour water, and potass extraction is also added into the impurity that is difficult to remove, adds the cost that the later stage processes, contaminated environment.The method of supercritical carbon dioxide extraction Folium Mori active substance, has and yields poorly, the shortcoming that product purity is not high, and energy consumption and investment are relatively big, are unfavorable for large-scale production.For the fresh mulberry leaf plucked, mostly adopting nature to dry method and process, in dry process, flavones content can be gradually lowered, and cured leaf can affect extracting flavonoids rate, and later stage extraction and purification all can produce impact.
Summary of the invention
It is an object of the invention to provide a kind of method extracting total flavonoid functional materials from Folium Mori, by Folium Mori being carried out lactic acid bacteria fermentation preservation, increasing production stability, reducing the loss of product.Folium Mori after lactic acid bacteria preservation, when being used further to extract flavones in mulberry leaves, extraction ratio is higher, and the lactic acid of lactic acid bacteria metabolism contributes to reducing production cost, use ultrafilter membrane during subsequent purification, while obtaining high-quality product, shorten the production time, reducing energy resource consumption, the exploitation for Folium Mori provide a kind of new method.
In order to reach above-mentioned purpose, the present invention adopts the following technical scheme that
A kind of method extracting total flavonoid functional materials from Folium Mori, carries out as follows:
A. clean: adopt deionized water that the fresh Folium Mori taken are carried out surface drip washing process；
B. preservation: the ratio mixing of the Folium Mori 1:1000-10000 in mass ratio after cleaning with step a with lactic acid bacteria, and preserve at sealing bag or cement pit anaerobic environment lower seal anaerobic fermentation, holding time >=7 days, maximum duration is 2 years；
C. extract: with the Folium Mori of water cleaning step b preservation, then by hydrochloric acid-deionized water under 80-100 DEG C of condition: the ratio mixing reflux, extract, 2-5h of Folium Mori=(6-30): 1 (volume: quality), filter, obtain flavones in mulberry leaves crude extract A.
D. refine: the flavones in mulberry leaves crude extract A of step c is first passed through the ultrafilter membrane of molecular weight 10000-50000Da, collect permeate；Permeate collects trapped fluid again through the ultrafilter membrane of molecular weight 100-500Da, and namely this trapped fluid concentrate drying obtains Folium Mori total flavonoids product.
The purpose of the present invention realizes also by following technical measures:
Lactic acid bacteria anaerobic fermentation natural environment temperature described in step b, natural pH.
The pH of hydrochloric acid-deionized water described in step c is 1-6.
When flavones in mulberry leaves crude extract described in step d crosses the ultrafilter membrane that molecular weight is 10000-50000Da, feed concentration 0.5%-3%, crosses film pressure 0.5-4MPa.Cross the ultrafilter membrane of molecular weight 100-500Da, feed concentration 0.5%-3%, cross film pressure 0.5-4MPa.
Described lactic acid bacteria is commercially available fruit and vegerable special lactobacillus preservative agent.
Described hydrochloric acid is food grade hydrochloric acid.
The present invention, compared with other techniques, has the advantage that
(1) present invention adopts lactic acid bacteria preservation Folium Mori to extract flavone, can solve Folium Mori pluck under because of can not in time subsequent production and produce each constituent content change affect end product quality, part glucide in Folium Mori can also be changed into lactic acid, improve flavone product purity, add the stability of integrated artistic, solve stickness shortcoming after flavones in mulberry leaves product drying.
(2) present invention adopts the Folium Mori that lactic acid bacteria preserves to extract flavone, growth metabolism due to lactic acid bacteria, Hui Shi plant cell tissue crushes, advantageously in the leaching of flavone, thus increasing extracting flavonoids rate (air-dry Folium Mori, fresh mulberry leaf and lactic acid bacteria preserve the extracting flavonoids rate of Folium Mori compare see accompanying drawing 1).The present invention adopts acid extraction simultaneously, the lactic acid that lactic acid bacteria metabolism generates, and has bigger contribution to reducing extracting solution pH, thus reducing hydrochloric acid consumption, saving cost, decreasing the pollution to environment simultaneously, open the new way that Folium Mori utilize, improve the medicinal rate of mulberry leaf resource and economic value added.
(3) flavones in mulberry leaves is purified by the device for ultrafiltration membrane that the present invention adopts, and adopts Using Multistage Membranes to retain separation purification, more traditional purification by macroporous resin technique, efficiency is high, constant product quality, saves the energy, simple to operate, environmental pollution is little, it is easier to industrialized production.
Accompanying drawing explanation
Fig. 1 is the comparison that air-dry Folium Mori, fresh mulberry leaf and lactic acid bacteria preserve flavones in mulberry leaves extraction ratio；
Fig. 2 is the process flow diagram of the inventive method.
Detailed description of the invention
Embodiment 1:
To the fresh Folium Mori deionized water drip washing taken, then the water on Folium Mori surface is drained, mix by the ratio of lactic acid bacteria Yu Folium Mori 1:5000 in mass ratio, and seal preservation 7 days, then with hydrochloric acid-deionized water that pH is 1, mix reflux, extract, 2h with Folium Mori in the ratio of 7:1 (volume: quality) and filter at 80 DEG C, make flavones in mulberry leaves extracting solution, the film of molecular weight 10000Da is finally first passed through with membrane separation plant, pressure is 1MPa, sample introduction liquid solid content is 1%, permeate is again through the film of molecular weight 100Da, pressure is 4MPa, now the solid concentration of feeding liquid is 0.5%, collect trapped fluid, finished product is obtained after trapped fluid concentrate drying, flavones content 28.65%.
Embodiment 2:
To the fresh Folium Mori deionized water drip washing taken, then the water on Folium Mori surface is drained, mix by the ratio of lactic acid bacteria Yu Folium Mori 1:8000 in mass ratio, and seal preservation 30 days, then with hydrochloric acid-deionized water that pH is 2, mix reflux, extract, 3h with Folium Mori in the ratio of 8:1 (volume: quality) and filter at 90 DEG C, make flavones in mulberry leaves extracting solution, the film of molecular weight 30000Da is finally first passed through with membrane separation plant, pressure is 1.5MPa, sample introduction liquid solid content is 2%, permeate is again through the film of molecular weight 200Da, pressure is 2.5MPa, collect trapped fluid, finished product is obtained after trapped fluid concentrate drying, recording flavones content is 30.18%.
Embodiment 3
To the fresh Folium Mori deionized water drip washing taken, then the water on Folium Mori surface is drained, mix by the ratio of lactic acid bacteria Yu Folium Mori 1:3000 in mass ratio, and sealing and fermenting preserves 1 year, then with hydrochloric acid-deionized water that pH is 6, mix reflux, extract, 4h with Folium Mori in the ratio of 10:1 (volume: quality) and filter at 98 DEG C, make flavones in mulberry leaves extracting solution, the film of molecular weight 50000Da is finally first passed through with membrane separation plant, pressure is 2MPa, sample introduction liquid solid content is 3%, the permeate film by molecular weight 300Da, pressure is 3MPa, the solid concentration of feed liquid is 2%, collect trapped fluid, finished product is obtained after concentrate drying, recording flavones content is 29.96%.
Embodiment 4
To the fresh Folium Mori deionized water drip washing taken, then the water on Folium Mori surface is drained, mix by the ratio of lactic acid bacteria Yu Folium Mori 1:1000 in mass ratio, seal and preserve half a year, then with hydrochloric acid-deionized water that pH is 3, mix reflux, extract, 4h with Folium Mori in the ratio of 6:1 (volume: quality) and filter at 100 DEG C, make flavones in mulberry leaves extracting solution, the film of molecular weight 20000Da is finally first passed through with membrane separation plant, pressure is 0.5MPa, sample introduction liquid solid content is 0.5%, the permeate film by molecular weight 400Da, pressure is 0.5MPa, collect trapped fluid, finished product is obtained after concentrate drying, recording flavones content is 26.62%.
Embodiment 5
To the fresh Folium Mori deionized water drip washing taken, then the water on Folium Mori surface is drained, mix by the ratio of lactic acid bacteria Yu Folium Mori 1:10000 in mass ratio, seal and preserve 200 days, then with hydrochloric acid-deionized water that pH is 5, mix reflux, extract, 5h with Folium Mori in the ratio of 30:1 (volume: quality) and filter at 90 DEG C, make flavones in mulberry leaves extracting solution, the film of molecular weight 40000Da is finally first passed through with membrane separation plant, pressure is 4MPa, sample introduction liquid solid content is 3%, permeate is again through the film of molecular weight 500Da, pressure is 4MPa, feeding liquid solid concentration is 3%, collect trapped fluid, finished product is obtained after trapped fluid concentrate drying, recording flavones content is 28.05%.
Claims (1)
1. the method extracting total flavonoid functional materials from Folium Mori, it is characterised in that
To the fresh Folium Mori deionized water drip washing taken, then the water on Folium Mori surface is drained, mix by the ratio of lactic acid bacteria Yu Folium Mori 1:8000 in mass ratio, and seal preservation 30 days, then with hydrochloric acid-deionized water that pH is 2, with Folium Mori in 8:1(volume at 90 DEG C: quality) ratio mix reflux, extract, 3h and filter, make flavones in mulberry leaves extracting solution, the film of molecular weight 30000Da is finally first passed through with membrane separation plant, pressure is 1.5MPa, sample introduction liquid solid content is 2%, permeate is again through the film of molecular weight 200Da, pressure is 2.5MPa, collect trapped fluid, finished product is obtained after trapped fluid concentrate drying, recording flavones content is 30.18%.
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| CN105560378A (en) * | 2015-12-29 | 2016-05-11 | 漯河医学高等专科学校 | New use of mulberry leaf total flavonoids |
| CN105616504A (en) * | 2016-03-01 | 2016-06-01 | 杭州蚕宝生物技术有限公司 | Method for extracting blood sugar reduction small molecule active components from folium mori |
| CN109645304B (en) * | 2018-12-28 | 2022-04-05 | 广东省农业科学院蚕业与农产品加工研究所 | Preparation method of mulberry leaf health food base material |
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| CN102524769A (en) * | 2011-11-04 | 2012-07-04 | 博仲盛景医药技术（北京）有限公司 | Mulberry leaf extractive and preparation method and application thereof |
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| CN102524769A (en) * | 2011-11-04 | 2012-07-04 | 博仲盛景医药技术（北京）有限公司 | Mulberry leaf extractive and preparation method and application thereof |
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| Title |
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| 饲料桑叶青贮法质量比较研究;马群忠等;《饲料研究》;20121231(第9期);77-79 * |
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