CN105399717A - Method for extracting flavones from rice bran - Google Patents
Method for extracting flavones from rice bran Download PDFInfo
- Publication number
- CN105399717A CN105399717A CN201510938674.0A CN201510938674A CN105399717A CN 105399717 A CN105399717 A CN 105399717A CN 201510938674 A CN201510938674 A CN 201510938674A CN 105399717 A CN105399717 A CN 105399717A
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- rice bran
- flavones
- extraction
- bran powder
- dry
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/40—Separation, e.g. from natural material; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a method for extracting flavones from rice bran. The method includes the following steps: 1) removing impurities of the rice bran, drying the rice bran, and crushing the dried rice bran; 2) carrying out enzymolysis of the crushed material, adding hot water, carrying out reflux extraction, filtering, and concentrating under reduced pressure to obtain a concentrate; and 3) separating and purifying the concentrate with macroporous resin, and thus obtaining the flavones extracts. The method has high extraction purity on the flavones in the rice bran, and has reliable data and simple extraction method. At the same time, requirements for equipment are low, intermediate products and final products are all non-toxic, the safety is high, the production cost is low, and the method is suitable for industrial production.
Description
Technical field
The present invention relates to the extractive technique of flavones.More specifically, a kind of method extracting flavones from rice bran is related to.
Background technology
Rice bran is processed into by seed coat and embryo, is the principal by product of paddy processing.Its quality accounts for 6% ~ 8% of whole paddy, and the output of the annual rice bran of China, up to 1,000 ten thousand more than t, occupies first of the world.Current rice bran still exists as the not high agricultural byproducts of utilization ratio in China's most area.Result of study both domestic and external and data show, are rich in various nutrient substance and physiologically active substance in rice bran.Because the raw material processing rice bran is different with adopted processing technology. the moiety of rice bran is not just the same.In general, average containing protein 15% in rice bran, fatty 16%-22%, sugared 3%-8%, moisture 10%, heat is approximately 125.1KJ/g.Lipid acid main in fat is mostly the unsaturated fatty acids such as oleic acid, linolic acid, and containing a large amount VITAMIN, pohytol, food fibre, amino acid and mineral substance etc.Have the title of " natural nutrition treasure-house ", rice bran contains a certain amount of flavonoid compound.
Flavones has the material of multiple physiologically active as a class, is not only applied in the exploitation of medicine and healthcare products, is also widely used in the industry such as makeup, food and feed additive.Show through large quantity research: flavones has significantly anti-ageing, hypoglycemic, anticancer, analgesia, anti-inflammatory, the effect such as antibacterial.
At present, rice bran is the principal by product of paddy processing, and a few part is utilized, great majority or be directly dropped, cause the serious wasting of resources.Do not obtain effectively and fully utilizing.
Summary of the invention
The technical problem to be solved in the present invention is the extracting method providing a kind of Rice Bran Flavonoid, and the flavones purity that this extracting method can make extraction obtain reaches more than 79.32%.
For achieving the above object, the present invention adopts following technical proposals:
From rice bran, extract a method for flavones, comprise the steps:
1) rice bran is crossed removal of impurities sieve, remove impurity, dry, pulverize through pulverizer, cross 80 mesh sieves, make rice bran powder;
2) rice bran powder is carried out enzymolysis, then to heating water refluxing extraction in product 2-3 time, filter, obtain yellow filtrate, then concentrate filtrate to dry;
3) with macroporous adsorbent resin to step 2) gained enriched material carries out wash-out separation and purification.
Preferably, step 1) in, the condition of described drying is dry 24-30h at 50-60 DEG C.
Preferably, step 2) in, described enzymolysis step is: in the aqueous solution of rice bran powder, add complex enzyme liquid, regulates the PH to 4-6 of mixture, at 45-55 DEG C of temperature, reacts 1-2h; The mass ratio of described rice bran powder and complex enzyme liquid is 25:1-35:2.
Preferably, in described complex enzyme liquid, prozyme is selected from one or more in cellulase, polygalacturonase or papoid, and damping fluid is selected from Tutofusin tris.
Preferably, step 2) in, each extraction time of described heating water refluxing extraction is 3-4h, and hot water temperature is 70-80 DEG C.
Preferably, step 3) in, described separation and purification comprises step 2) gains first carry out Static Adsorption, then carry out dynamic adsorption; The condition of described dynamic adsorption is: sample solution is step 2) aqueous solution of gains, mass concentration is 7-8mg/mL; Loading flow velocity is 3mL/min, and applied sample amount is 2 ~ 3 times of column volumes, with the washed resin of 2 ~ 3 times of column volumes after loading, then uses the ethanol elution of 70-80%, elution speed 3mL/min.
Macroporous adsorbent resin in the present invention can be selected from the D101 type macroporous adsorbent resin that Tianjin Hao Ju resin Science and Technology Ltd. produces.In the present invention, macroporous adsorbent resin is under this extracting method, reusable 7-9 time, and service efficiency is high.Simultaneously, in the present invention, rice bran powder and prozyme are carried out composite, to the kind of prozyme and and the consumption of rice bran powder carry out strict restriction, make the sufficient enzymolysis of rice bran powder, heating and refluxing extraction is carried out again after enzymolysis, further ensure that the biological activity of enzyme, make enzymolysis complete, the flavones purity of extraction is high.Simultaneously in the present invention, heating and refluxing extraction is simple to the requirement of equipment, and data are reliable, reduces investment outlay, reduces costs, security is high.
Beneficial effect of the present invention is as follows:
The purity of the present invention to the extraction of flavones in rice bran is high, and data are reliable, and extracting method is simple.
Requirement to equipment of the present invention is low, and intermediate product and end product are all nontoxic, and security is high, and production cost is low, is applicable to industrial production.
Embodiment
In order to be illustrated more clearly in the present invention, below in conjunction with preferred embodiment, the present invention is described further.It will be appreciated by those skilled in the art that specifically described content is illustrative and nonrestrictive, should not limit the scope of the invention with this below.
Embodiment 1
From rice bran, extract a method for flavones, comprise the steps:
1) rice bran is crossed removal of impurities sieve, remove impurity, dry 30h at 50 DEG C of temperature, then shatter process through pulverizer, cross 80 mesh sieves, obtain rice bran powder;
2) in the aqueous solution of above-mentioned gained rice bran powder, cellulase solution is added, wherein the mass ratio of rice bran powder and cellulase solution is 25:1,2h is reacted at 45 DEG C of temperature, obtain product, in product, add 70 DEG C of hot water, refluxing extraction 2 times, each time is 4h, filter, obtain yellow filtrate, concentrate filtrate to dry;
3) with D101 type macroporous adsorbent resin to step 2) enriched material carries out wash-out separation and purification, first carry out carrying out Static Adsorption to enriched material, adsorption time is 15min, carry out dynamic adsorption again, dynamic adsorption condition is: selecting mass concentration to be the enriched material aqueous solution of 7mg/mL is sample solution, loading flow velocity is 3mL/min, and applied sample amount is 2 times of column volumes, and the dynamic adsorption time is 4min; With the washed resin of 2 times of column volumes after loading, then use the ethanol elution of 70%, elution speed 3mL/min.
After the separation and purification of macroporous resin wash-out, namely complete the extraction of flavones in rice bran, the flavones purity 82.1% of extraction.
Embodiment 2
From rice bran, extract a method for flavones, comprise the steps:
1) rice bran is crossed removal of impurities sieve, remove impurity, dry 24h at 60 DEG C of temperature, then shatter process through pulverizer, cross 80 mesh sieves, obtain rice bran powder;
2) in the aqueous solution of above-mentioned gained rice bran powder, cellulase solution is added, wherein the mass ratio of rice bran powder and cellulase solution is 35:2,1h is reacted at 55 DEG C of temperature, obtain product, in product, add 80 DEG C of hot water, refluxing extraction 3 times, each time is 3h, filter, obtain yellow filtrate, concentrate filtrate to dry;
3) with D101 type macroporous adsorbent resin to step 2) enriched material carries out wash-out separation and purification, first carry out carrying out Static Adsorption to enriched material, adsorption time is 15min, carry out dynamic adsorption again, dynamic adsorption condition is: selecting mass concentration to be the enriched material aqueous solution of 8mg/mL is sample solution, loading flow velocity is 3mL/min, and applied sample amount is 2 times of column volumes, and the dynamic adsorption time is 4min; With the washed resin of 2 times of column volumes after loading, then use the ethanol elution of 80%, elution speed 3mL/min.
After the separation and purification of macroporous resin wash-out, namely complete the extraction of flavones in rice bran, the flavones purity 79.32% of extraction.
Embodiment 3
Repeat embodiment 1, difference is, by step 2) cellulase changes polygalacturonase into, and all the other conditions are constant, complete the extraction of flavones in rice bran, the flavones purity 83.4% of extraction.
Embodiment 4
Repeat embodiment 1, difference is, by step 2) cellulase changes papoid into, and all the other conditions are constant, complete the extraction of flavones in rice bran, the flavones purity 86.6% of extraction.
Obviously; the above embodiment of the present invention is only for example of the present invention is clearly described; and be not the restriction to embodiments of the present invention; for those of ordinary skill in the field; can also make other changes in different forms on the basis of the above description; here cannot give exhaustive to all embodiments, every belong to technical scheme of the present invention the apparent change of extending out or variation be still in the row of protection scope of the present invention.
Claims (6)
1. from rice bran, extract a method for flavones, it is characterized in that, comprise the steps:
1) rice bran is crossed removal of impurities sieve, remove impurity, dry, pulverize through pulverizer, cross 80 mesh sieves, make rice bran powder;
2) rice bran powder is carried out enzymolysis, then to heating water refluxing extraction in product 2-3 time, filter, obtain yellow filtrate, then concentrate filtrate to dry;
3) with macroporous adsorbent resin to step 2) gained enriched material carries out wash-out separation and purification.
2. method according to claim 1, is characterized in that, step 1) in, the condition of described drying is dry 24-30h at 50-60 DEG C.
3. method according to claim 1, is characterized in that, step 2) in, described enzymolysis step is: in the aqueous solution of rice bran powder, add complex enzyme liquid, regulates the PH to 4-6 of mixture, at 45-55 DEG C of temperature, reacts 1-2h; The mass ratio of described rice bran powder and complex enzyme liquid is 25:1-35:2.
4. method according to claim 3, is characterized in that, in described complex enzyme liquid, prozyme is selected from one or more in cellulase, polygalacturonase or papoid, and damping fluid is selected from Tutofusin tris.
5. method according to claim 1, is characterized in that, step 2) in, each extraction time of described heating water refluxing extraction is 3-4h, and hot water temperature is 70-80 DEG C.
6. method according to claim 1, is characterized in that, step 3) in, described separation and purification comprises step 2) gains first carry out Static Adsorption, then carry out dynamic adsorption; The condition of described dynamic adsorption is: sample solution is step 2) aqueous solution of gains, mass concentration is 7-8mg/mL; Loading flow velocity is 3mL/min, and applied sample amount is 2 ~ 3 times of column volumes, with the washed resin of 2 ~ 3 times of column volumes after loading, then uses the ethanol elution of 70-80%, elution speed 3mL/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510938674.0A CN105399717A (en) | 2015-12-16 | 2015-12-16 | Method for extracting flavones from rice bran |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510938674.0A CN105399717A (en) | 2015-12-16 | 2015-12-16 | Method for extracting flavones from rice bran |
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| CN105399717A true CN105399717A (en) | 2016-03-16 |
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| CN201510938674.0A Pending CN105399717A (en) | 2015-12-16 | 2015-12-16 | Method for extracting flavones from rice bran |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106983830A (en) * | 2017-05-22 | 2017-07-28 | 辽宁大学 | Antidepression health products containing Rice Bran Flavonoid |
| CN109907319A (en) * | 2019-03-12 | 2019-06-21 | 中南林业科技大学 | A kind of rice bran extract and preparation method thereof and the application in health food |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102948758A (en) * | 2012-11-26 | 2013-03-06 | 陕西科技大学 | Method for extracting buckwheat flavone from buckwheat bran |
| CN104491510A (en) * | 2014-12-03 | 2015-04-08 | 吉林省标达科技有限责任公司 | Method for extracting total flavonoids from rice bran |
-
2015
- 2015-12-16 CN CN201510938674.0A patent/CN105399717A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102948758A (en) * | 2012-11-26 | 2013-03-06 | 陕西科技大学 | Method for extracting buckwheat flavone from buckwheat bran |
| CN104491510A (en) * | 2014-12-03 | 2015-04-08 | 吉林省标达科技有限责任公司 | Method for extracting total flavonoids from rice bran |
Non-Patent Citations (2)
| Title |
|---|
| 吴佳佳等: "米糠总黄酮提取工艺的研究", 《科学技术与工程》 * |
| 徐竞: "米糠黄酮的逆流提取工艺优化研究", 《粮食加工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106983830A (en) * | 2017-05-22 | 2017-07-28 | 辽宁大学 | Antidepression health products containing Rice Bran Flavonoid |
| CN109907319A (en) * | 2019-03-12 | 2019-06-21 | 中南林业科技大学 | A kind of rice bran extract and preparation method thereof and the application in health food |
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Application publication date: 20160316 |