CN104189087A - Method for extracting total flavonoid functional substance from folium mori - Google Patents
Method for extracting total flavonoid functional substance from folium mori Download PDFInfo
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- CN104189087A CN104189087A CN201410395997.5A CN201410395997A CN104189087A CN 104189087 A CN104189087 A CN 104189087A CN 201410395997 A CN201410395997 A CN 201410395997A CN 104189087 A CN104189087 A CN 104189087A
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Abstract
The invention provides a method for extracting a total flavonoid functional substance from folium mori, and belongs to the technical field of extracting and separating of natural products. The method comprises the following steps: a, washing, namely, leaching the surface of folium mori to remove dust on the folium mori; b, storage, namely, uniformly mixing lactic acid bacteria and folium mori leached in the step a based on the proportion, and then sealing and storing by an anaerobic fermentation manner through a sealing bag or a cement pit; c, extracting, namely, washing the folium mori stored in the step b with water, then mixing hydrochloric acid-deionized water and folium mori according to proportion, refluxing and extracting, and filtering to obtain a folium mori flavone crude extracting liquid A; d, fine preparing, namely, enabling the folium mori flavone crude extracting liquid A to pass through an ultrafiltration membrane with molecular weight of 10,000-50,000Da, collecting a permeating liquid, collecting an intercepted liquid through the ultrafiltration membrane with the molecular weight of 100-500Da, concentrating the intercepted liquid, and then spraying and drying to obtain a folium mori total flavonoid product. According to the method, lactic acid bacteria is used for storing folium mori extracting flavone; compared with the traditional method of extracting flavone from fresh or dry folium mori, the method has the advantages that the extracting rate of folium mori flavone can be greatly raised; meanwhile, the contents of macromolecule sugar and protein in the product can be decreased, and the purity of the product is improved; and in terms of purification of flavone, the ultrafiltration membrane technology is utilized to purify the folium mori flavone, which improves the energy conservation and environmental protection as compared with the process of purifying through macroreticular resin.
Description
Technical field
The present invention relates to natural product extraction and separation technology field, particularly a kind of method of lactobacillus preservation high efficiency extraction total flavonoid functional materials for Folium Mori.
Background technology
China mulberry of a great variety, has the cultivation of mulberry in southern and northern most areas.Folium Mori are primary products of mulberry, but Application and Development is less at present, mostly as offal treatment, causes resource greatly to waste.Find by pharmacological research, the flavonoid bioactive substance containing in Folium Mori is preventing and is treating the aspects such as diabetes, hypertension, hyperlipidemia and antiviral, defying age, anti-inflammation have the effect of highly significant.If its medicine resource is made full use of, the benefit of its economy and society is by considerable so.
At present, about the existing more Patents of extraction and purification of Folium Mori functional materials, as CN101412703A discloses a kind of method coproduction of mulberry tea flavone that utilizes ethanol water to cross resin, polysaccharide and alkaloidal composite extracting technique, CN101862372A discloses a kind of technique of utilizing aqueous alkali heating extraction and crossing the method production flavones in mulberry leaves of macroporous resin, and CN1762428 discloses the method for utilizing supercritical carbon dioxide to extract deoxidation nojirimycin Alkaloid and two kinds of effective ingredient of flavone from Folium Mori.Above patent is that extractant mostly is ethanol in Folium Mori, one or more have the extraction of bioactive substance, and extraction time is long, and cost is higher, flavone purification mostly adopts macroporous adsorbent resin, although this technique can improve flavone purity, all consumes larger to material and the energy.Potass extraction shell-broken effect is not as sour water, and potass extraction also added the impurity that is difficult to remove, and increased the cost of post-processed, 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 relatively large, be unfavorable for large-scale production.For the fresh mulberry leaf of plucking, mostly adopt nature to dry method processing, in dry process, flavones content can reduce gradually, and cured leaf can affect flavone extraction ratio, all can exert an influence to later stage extraction and purification.
Summary of the invention
The object of this invention is to provide a kind of method of extracting total flavonoid functional materials from Folium Mori, by Folium Mori are carried out to lactic acid bacteria fermentation preservation, increase production stability, reduce the loss of product.Folium Mori after lactobacillus preservation, while being used further to extract flavones in mulberry leaves, extraction ratio is higher, and the lactic acid of lactobacillus metabolism contributes to reduce production costs, when subsequent purification, use ultrafilter membrane, in obtaining high-quality product, shortened the production time, reduce energy resource consumption, for the exploitation of Folium Mori provide a kind of new method.
In order to reach above-mentioned purpose, the present invention adopts following technical scheme:
From Folium Mori, extract a method for total flavonoid functional materials, carry out as follows:
A. clean: adopt deionized water to carry out surperficial drip washing processing to the fresh Folium Mori of taking;
B. preservation: the Folium Mori after cleaning with lactobacillus and the step a in mass ratio ratio of 1:1000-10000 mix, and preserve at sealing bag or cement pit anaerobic environment lower seal anaerobic fermentation, holding time >=7 day, maximum duration is 2 years;
C. extract: the Folium Mori of water cleaning step b preservation, then under 80-100 DEG C of condition by hydrochloric acid-deionized water: Folium Mori=(6-30): the ratio of 1 (volume: quality) is mixed reflux, extract, 2-5h, filter, obtain flavones in mulberry leaves crude extract A.
D. refining: the flavones in mulberry leaves crude extract A of step c, first by the ultrafilter membrane of molecular weight 10000-50000Da, is collected to permeate; Permeate is collected trapped fluid by the ultrafilter membrane of molecular weight 100-500Da again, and this trapped fluid concentrate drying obtains Folium Mori total flavonoids product.
Object of the present invention also can realize by following technical measures:
Lactobacillus anaerobic fermentation natural environment temperature described in step b, natural pH.
Described in step c, the pH of hydrochloric acid-deionized water is 1-6.
When described in steps d, flavones in mulberry leaves crude extract is crossed molecular weight and is the ultrafilter membrane of 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%, crosses film pressure 0.5-4MPa.
Described lactobacillus 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 following advantage:
(1) the present invention adopts lactobacillus preservation Folium Mori to extract flavone, can solve under Folium Mori harvesting and affect end product quality because each constituent content that subsequent production produces in time changes, also part glucide in Folium Mori can be changed into lactic acid, improve flavone product purity, increase the stability of integrated artistic, solved stickness shortcoming after flavones in mulberry leaves product drying.
(2) the present invention adopts the Folium Mori that lactobacillus is preserved to extract flavone, due to the growth metabolism of lactobacillus, the fragmentation of Hui Shi plant cell tissue, more be conducive to the leaching of flavone, thereby increase flavone extraction ratio (air-dry Folium Mori, fresh mulberry leaf and lactobacillus are preserved the flavone extraction ratio of Folium Mori and relatively seen accompanying drawing 1).The present invention simultaneously adopts acid extraction, and the lactic acid that lactobacillus metabolism generates has larger contribution to reducing extracting solution pH, thereby reduce hydrochloric acid consumption, cost-saving, reduced the pollution to environment simultaneously, open up the new way that Folium Mori utilize, improved the medicinal rate of Folium Mori resource and economic value added.
(3) device for ultrafiltration membrane that the present invention adopts carries out purification to flavones in mulberry leaves, adopts Using Multistage Membranes to hold back separation and purification, more traditional purification by macroporous resin technique, efficiency is high, constant product quality, energy savings, simple to operate, environmental pollution is little, is easier to suitability for industrialized production.
Brief description of the drawings
Fig. 1 is the comparison that air-dry Folium Mori, fresh mulberry leaf and lactobacillus are preserved 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 of taking deionized water drip washing, then drain the water on Folium Mori surface, with lactobacillus and Folium Mori in mass ratio the ratio of 1:5000 mix, and sealing is preserved 7 days, then hydrochloric acid-the deionized water that is 1 with pH, at 80 DEG C, mix reflux, extract, 2h and filter in the ratio of 7:1 (volume: quality) with Folium Mori, make flavones in mulberry leaves extracting solution, finally first pass through the film of molecular weight 10000Da with membrane separation plant, pressure is 1MPa, sample introduction liquid solid content is 1%, permeate is again by the film of molecular weight 100Da, pressure is 4MPa, now the solid concentration of feeding liquid is 0.5%, collect trapped fluid, after trapped fluid concentrate drying, obtain finished product, flavones content 28.65%.
Embodiment 2:
To the fresh Folium Mori of taking deionized water drip washing, then drain the water on Folium Mori surface, with lactobacillus and Folium Mori in mass ratio the ratio of 1:8000 mix, and sealing is preserved 30 days, then hydrochloric acid-the deionized water that is 2 with pH, at 90 DEG C, mix reflux, extract, 3h and filter in the ratio of 8:1 (volume: quality) with Folium Mori, make flavones in mulberry leaves extracting solution, finally first pass through the film of molecular weight 30000Da with membrane separation plant, pressure is 1.5MPa, sample introduction liquid solid content is 2%, permeate is again by the film of molecular weight 200Da, pressure is 2.5MPa, collect trapped fluid, after trapped fluid concentrate drying, obtain finished product, recording flavones content is 30.18%.
Embodiment 3
To the fresh Folium Mori of taking deionized water drip washing, then drain the water on Folium Mori surface, with lactobacillus and Folium Mori in mass ratio the ratio of 1:3000 mix, and sealing and fermenting is preserved 1 year, then hydrochloric acid-the deionized water that is 6 with pH, at 98 DEG C, mix reflux, extract, 4h and filter in the ratio of 10:1 (volume: quality) with Folium Mori, make flavones in mulberry leaves extracting solution, finally first pass through the film of molecular weight 50000Da with membrane separation plant, pressure is 2MPa, sample introduction liquid solid content is 3%, permeate is by the film of molecular weight 300Da, pressure is 3MPa, the solid concentration of feed liquid is 2%, collect trapped fluid, after concentrate drying, obtain finished product, recording flavones content is 29.96%.
Embodiment 4
To the fresh Folium Mori of taking deionized water drip washing, then drain the water on Folium Mori surface, with lactobacillus and Folium Mori in mass ratio the ratio of 1:1000 mix, half a year is preserved in sealing, then hydrochloric acid-the deionized water that is 3 with pH, at 100 DEG C, mix reflux, extract, 4h and filter in the ratio of 6:1 (volume: quality) with Folium Mori, make flavones in mulberry leaves extracting solution, finally first pass through the film of molecular weight 20000Da with membrane separation plant, pressure is 0.5MPa, sample introduction liquid solid content is 0.5%, permeate is by the film of molecular weight 400Da, pressure is 0.5MPa, collect trapped fluid, after concentrate drying, obtain finished product, recording flavones content is 26.62%.
Embodiment 5
To the fresh Folium Mori of taking deionized water drip washing, then drain the water on Folium Mori surface, with lactobacillus and Folium Mori in mass ratio the ratio of 1:10000 mix, sealing is preserved 200 days, then hydrochloric acid-the deionized water that is 5 with pH, at 90 DEG C, mix reflux, extract, 5h and filter in the ratio of 30:1 (volume: quality) with Folium Mori, make flavones in mulberry leaves extracting solution, finally first pass through the film of molecular weight 40000Da with membrane separation plant, pressure is 4MPa, sample introduction liquid solid content is 3%, permeate is again by the film of molecular weight 500Da, pressure is 4MPa, feeding liquid solid concentration is 3%, collect trapped fluid, after trapped fluid concentrate drying, obtain finished product, recording flavones content is 28.05%.
Claims (4)
1. a method of extracting total flavonoid functional materials from Folium Mori, is characterized in that, carries out as follows:
A. clean: adopt deionized water to carry out surperficial drip washing processing to the fresh Folium Mori of taking;
B. preservation: the Folium Mori after cleaning with lactobacillus and the step a in mass ratio ratio of 1:1000-10000 mix, and preserve at sealing bag or cement pit anaerobic environment lower seal anaerobic fermentation, holding time >=7 day, maximum duration is 2 years;
C. extract: the Folium Mori of water cleaning step b preservation, then under 80-100 DEG C of condition by hydrochloric acid-deionized water: Folium Mori=(6-30): the ratio of 1 (volume: quality) is mixed reflux, extract, 2-5h, filter, obtain flavones in mulberry leaves crude extract A;
D. refining: the flavones in mulberry leaves crude extract A of step c, first by the ultrafilter membrane of molecular weight 10000-50000Da, is collected to permeate; Permeate is collected trapped fluid by the ultrafilter membrane of molecular weight 100-500Da again, and trapped fluid obtains Folium Mori total flavonoids product through concentrate drying.
2. a kind of method of extracting total flavonoid functional materials from Folium Mori claimed in claim 1, is characterized in that, lactobacillus anaerobic fermentation described in step b, natural environment temperature, natural pH.
3. a kind of method of extracting total flavonoid functional materials from Folium Mori as claimed in claim 1, is characterized in that, the pH of hydrochloric acid-deionized water is 1-6 described in step c.
4. a kind of method of extracting total flavonoid functional materials from Folium Mori as claimed in claim 1, is characterized in that, when crude extract is crossed molecular weight and is the ultrafilter membrane of 10000-50000Da described in steps d, crossing film concentration is 0.5%-3%, crosses film pressure 0.5-4MPa; When described permeate is crossed the ultrafilter membrane of molecular weight 100-500Da, the concentration of feeding liquid is 0.5%-3%, crosses film pressure 0.5-4MPa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109645304A (en) * | 2018-12-28 | 2019-04-19 | 广东省农业科学院蚕业与农产品加工研究所 | A kind of preparation method of mulberry leaf material for healthy food |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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- 2014-08-12 CN CN201410395997.5A patent/CN104189087B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 马群忠等: "饲料桑叶青贮法质量比较研究", 《饲料研究》, no. 9, 31 December 2012 (2012-12-31), pages 77 - 79 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109645304A (en) * | 2018-12-28 | 2019-04-19 | 广东省农业科学院蚕业与农产品加工研究所 | A kind of preparation method of mulberry leaf material for healthy food |
| 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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