CN103965154A - Method for producing soybean isoflavone by utilizing soybean molasses - Google Patents
Method for producing soybean isoflavone by utilizing soybean molasses Download PDFInfo
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- CN103965154A CN103965154A CN201410194447.7A CN201410194447A CN103965154A CN 103965154 A CN103965154 A CN 103965154A CN 201410194447 A CN201410194447 A CN 201410194447A CN 103965154 A CN103965154 A CN 103965154A
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- molasses
- paste
- soybean
- soybean isoflavones
- diluted
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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
- C07D311/34—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 3 only
- C07D311/36—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 3 only not hydrogenated in the hetero ring, e.g. isoflavones
-
- 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
Abstract
The invention relates to a method for producing soybean isoflavone by utilizing soybean molasses. The method comprises the following step of extracting the soybean molasses through dilution, acid treatment, heat treatment, column chromatography, crystallization, drying and other processes, wherein the content of the obtained soybean isoflavone is more than 40 percent. The method has the benefits that as the soybean isoflavone is extracted by utilizing the soybean molasses as a by-product of an alcohol leaching soy protein concentrate, the added value of the soybean molasses is greatly increased; the method is suitable for industrial production.
Description
Technical field
The present invention relates to the production of high-content soybean isoflavones, refer in particular to the method for utilizing soy molasses to produce soybean isoflavones.
Background technology
Soybean isoflavones is mainly present in various leguminous plantss, and soybean is the topmost dietary source of soybean isoflavones.Soybean isoflavones has the molecular structure similar to oestrogenic hormon, can with women's body in oestrogenic hormon competitive binding estrogen receptor, thereby reach the effect of two-ways regulation women body inner estrogen level.Research shows, soybean isoflavones has more outstanding effect at aspects such as improving Menopause, osteoporosis, cardiovascular disorder.
Soy molasses is the byproduct that alcohol method is produced soybean protein concentrate, and wherein the content of soybean isoflavones is 1%～2%.At present soy molasses is mainly for the production of the auxiliary material of feed, utilizes insufficiently, and added value is low.The present invention utilizes soy molasses to produce soybean isoflavones, saves soybean resource, improves the added value of soybean.
Publication number is the Chinese patent of CN1211573A, its production method is for take dregs of beans as raw material, utilize two one-step hydrolysis to produce soybean isoflavone aglycones product, publication number is the Chinese patent of CN1349987, its production method is raw material for take dregs of beans or plumule, through methanol extraction, flocculation, then utilize chromatography to refine purity higher than 50% soybean isoflavones product, publication number is the Chinese patent of CN1284503A, its production method, for take dregs of beans as raw material is through three counter-current extractions, then utilizes chromatography to carry out the soybean isoflavones product of purification of high-purity.
It is raw material that above three kinds of methods all adopt dregs of beans, exists following deficiency:
1, take dregs of beans as raw material production soybean isoflavones, when complex manufacturing, particularly lixiviate, extraction, use a large amount of organic solvents, while reclaiming solvent, energy consumption is large, and production cost is high.
2, take dregs of beans as raw material production soybean isoflavones, generally adopt methyl alcohol as vat liquor, the residual safety issue causing of methyl alcohol, is restricted the soybean isoflavones product of its production and the application of the residual dregs of rice of byproduct in production process.
3, take dregs of beans as raw material production soybean isoflavones, taken valuable soybean resource, and the isoflavone content in dregs of beans is very low, extract difficulty large, production process is difficult to control.
Summary of the invention
Object of the present invention is exactly to provide a kind of raising soybean added value for the deficiency of the method for above-mentioned existing production soybean isoflavones, saves soybean resource, reduces production costs, and utilizes soy molasses to produce the method for soybean isoflavones.
Technological process of the present invention is as follows:
(1), dilution: water is diluted to diluted molasses by soy molasses, and the sugar degree of diluted molasses is controlled at 8%～15%;
(2), acid is heavy: mineral acid is added in diluted molasses, regulate pH value to 2.5～4.5 of diluted molasses;
(3), thermal treatment: the diluted molasses of adjusting pH value is heated to 40 ℃～90 ℃ of temperature, is incubated and is cooled to room temperature after 30-120 minute;
(4), solid-liquid separation: by heat treated diluted molasses centrifugation, separate and subside thing and clear liquid;
(5), column chromatography: with column chromatography, isolated clear liquid is carried out to purifying, column chromatography filler is polystyrene low-pole macroporous resin, carries out drip washing with alcohol, and ethanol concn is 40%～90%, ambient operation;
(6), alcohol reclaims: column chromatography alcohol leacheate is carried out to negative pressure and be concentrated into paste, negative pressure thickening temperature is 60 ℃～90 ℃, and vacuum tightness is 0.02MPa～0.06MPa, and in paste, solid content is 20%～40%;
(7), crystallization: the solvent crystallization of 5～20 times of volumes for paste, standing sedimentation, collection supernatant liquor;
(8), solvent recuperation: by supernatant liquor negative pressure evaporation, reclaim solvent, obtain soybean isoflavones paste;
(9), dry: by soybean isoflavones paste at vacuum tightness 0.02 MPa～0.06MPa, temperature 70 C～90 ℃ dry 5～12 hours, to pulverize to obtain soy isoflavone solid powder.
Paste crystallization solvent used is 95% alcohol.
The heavy mineral acid used of acid is hydrochloric acid, sulfuric acid or phosphoric acid.
Solid-liquid separation is to adopt horizontal spiral centrifuge, tubular-bowl centrifuge or decanter type tripod pendulum type batch centrifugal.
The present invention utilizes soy molasses to produce the method for soybean isoflavones, has not only shortened operational path, has reduced production cost, saved the soybean resource of a large amount of preciousnesses, and fixed investment is little, simple to operate, is suitable for suitability for industrialized production.
Embodiment
Technological process of the present invention is as follows:
(1), dilution: water is diluted to diluted molasses by soy molasses, and the sugar degree of diluted molasses is controlled at 8%～15%;
(2), acid is heavy: mineral acid is added in diluted molasses, regulate pH value to 2.5～4.5 of diluted molasses;
(3), thermal treatment: the diluted molasses of adjusting pH value is heated to 40 ℃～90 ℃ of temperature, is incubated and is cooled to room temperature after 30-120 minute;
(4), solid-liquid separation: by heat treated diluted molasses centrifugation, separate and subside thing and clear liquid;
(5), column chromatography: with column chromatography, isolated clear liquid is carried out to purifying, column chromatography filler is polystyrene low-pole macroporous resin, carries out drip washing with alcohol, and ethanol concn is 40%～90%, ambient operation;
(6), alcohol reclaims: column chromatography alcohol leacheate is carried out to negative pressure and be concentrated into paste, negative pressure thickening temperature is 60 ℃～90 ℃, and vacuum tightness is 0.02MPa～0.06MPa, and in paste, solid content is 20%～40%;
(7), crystallization: the solvent crystallization of 5～20 times of volumes for paste, standing sedimentation, collection supernatant liquor;
(8), solvent recuperation: by supernatant liquor negative pressure evaporation, reclaim solvent, obtain soybean isoflavones paste;
(9), dry: by soybean isoflavones paste at vacuum tightness 0.02 MPa～0.06MPa, temperature 70 C～90 ℃ dry 5～12 hours, to pulverize to obtain soy isoflavone solid powder.
Paste crystallization solvent used is 95% alcohol.
The heavy mineral acid used of acid is hydrochloric acid, sulfuric acid or phosphoric acid.
Solid-liquid separation is to adopt horizontal spiral centrifuge, tubular-bowl centrifuge or decanter type tripod pendulum type batch centrifugal.
Embodiment 1:
Get 1000L soy molasses, thin up, regulating the sugar degree of diluted molasses water is 10%.Slowly add while stirring 1N hydrochloric acid soln, regulating the pH value of diluted molasses water is 3.8.Be heated to 65 ℃, be incubated and be cooled to room temperature after 60 minutes.Centrifugal with decanter type tripod pendulum type batch centrifugal, collect centrifugal clear liquid and carry out column chromatography, with 70% spirituous solution drip washing.Collect leacheate, negative pressure evaporation, vaporization temperature is 70 ℃, and vacuum tightness is 0.02MPa, and recovered alcohol obtains solid content and is 25% soybean isoflavones paste.95% alcohol toward adding 8 times of volumes in soybean isoflavones paste, stirs standing sedimentation 30 minutes.Collect supernatant liquor, negative pressure recovered alcohol, obtains soybean isoflavones paste.By soybean isoflavones paste at 80 ℃ of vacuum tightness 0.02MPa, temperature dry 8 hours, grind, obtain 4528 grams of soybean isoflavones, purity is 51.26%.
Embodiment 2:
Get 1000L soy molasses, thin up, regulating the sugar degree of diluted molasses water is 15%.Slowly add while stirring 1N sulphuric acid soln, regulating the pH value of diluted molasses water is 4.2.Be heated to 80 ℃, be incubated and be cooled to room temperature after 90 minutes.Centrifugal with tubular-bowl centrifuge, collect centrifugal clear liquid and carry out column chromatography, with 75% spirituous solution drip washing.Collect leacheate, negative pressure evaporation, vaporization temperature is 70 ℃, and vacuum tightness is 0.02MPa, and recovered alcohol obtains solid content and is 28% soybean isoflavones paste.95% alcohol toward adding 10 times of volumes in soybean isoflavones paste, stirs standing sedimentation 30 minutes.Collect supernatant liquor, negative pressure recovered alcohol, obtains soybean isoflavones paste.By soybean isoflavones paste at 80 ℃ of vacuum tightness 0.02MPa, temperature dry 4 hours, grind, obtain 4636 grams of soybean isoflavones, purity is 54.55%.
Claims (4)
1. utilize soy molasses to produce a method for soybean isoflavones, it is characterized in that technological process is as follows:
(1), dilution: water is diluted to diluted molasses by soy molasses, and the sugar degree of diluted molasses is controlled at 8%～15%;
(2), acid is heavy: mineral acid is added in diluted molasses, regulate pH value to 2.5～4.5 of diluted molasses;
(3), thermal treatment: the diluted molasses of adjusting pH value is heated to 40 ℃～90 ℃ of temperature, is incubated and is cooled to room temperature after 30～120 minutes;
(4), solid-liquid separation: by heat treated diluted molasses centrifugation, separate and subside thing and clear liquid;
(5), column chromatography: with column chromatography, isolated clear liquid is carried out to purifying, column chromatography filler is polystyrene low-pole macroporous resin, carries out drip washing with alcohol, and ethanol concn is 40%～90%, ambient operation;
(6), alcohol reclaims: column chromatography alcohol leacheate is carried out to negative pressure and be concentrated into paste, negative pressure thickening temperature is 60 ℃～90 ℃, and vacuum tightness is 0.02MPa～0.06MPa, and in paste, solid content is 20%～40%;
(7), crystallization: the solvent crystallization of 5～20 times of volumes for paste, standing sedimentation, collection supernatant liquor;
(8), solvent recuperation: by supernatant liquor negative pressure evaporation, reclaim solvent, obtain soybean isoflavones paste;
(9), dry: by soybean isoflavones paste at vacuum tightness 0.02 MPa～0.06MPa, temperature 70 C～90 ℃ dry 5～12 hours, to pulverize to obtain soy isoflavone solid powder.
2. the method for utilizing soy molasses to produce soybean isoflavones according to claim 1, is characterized in that, paste crystallization solvent used is 95% alcohol.
3. the method for utilizing soy molasses to produce soybean isoflavones according to claim 1, is characterized in that, the heavy mineral acid used of acid is hydrochloric acid, sulfuric acid or phosphoric acid.
4. the method for utilizing soy molasses to produce soybean isoflavones according to claim 1, is characterized in that, solid-liquid separation is to adopt horizontal spiral centrifuge, tubular-bowl centrifuge or decanter type tripod pendulum type batch centrifugal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410194447.7A CN103965154B (en) | 2014-05-09 | 2014-05-09 | A kind of method utilizing soy molasses to produce soybean isoflavones |
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| CN201410194447.7A CN103965154B (en) | 2014-05-09 | 2014-05-09 | A kind of method utilizing soy molasses to produce soybean isoflavones |
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| CN103965154A true CN103965154A (en) | 2014-08-06 |
| CN103965154B CN103965154B (en) | 2015-10-14 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108203445A (en) * | 2017-11-20 | 2018-06-26 | 荆门市德爱生物工程股份有限公司 | A kind of method using soy molasses production soybean lecithin |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1174839A (en) * | 1996-06-11 | 1998-03-04 | 蛋白质技术国际公司 | Recovery of isoflavones from soy molasses |
| US6083553A (en) * | 1998-06-05 | 2000-07-04 | Protein Technologies International, Inc. | Recovery of isoflavones from soy molasses |
| CN101063158A (en) * | 2007-05-18 | 2007-10-31 | 东北农业大学 | Method for preparing soybean isoflavone aglycone |
| CN101824019A (en) * | 2009-12-17 | 2010-09-08 | 山东万得福实业集团有限公司 | Method for extracting isoflavone from soyabean molasses |
| CN103342691A (en) * | 2013-07-09 | 2013-10-09 | 内蒙古科然生物高新技术有限责任公司 | Method and equipment for extracting isoflavone, saponin and oligosaccharide from soy molasses |
-
2014
- 2014-05-09 CN CN201410194447.7A patent/CN103965154B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1174839A (en) * | 1996-06-11 | 1998-03-04 | 蛋白质技术国际公司 | Recovery of isoflavones from soy molasses |
| US6083553A (en) * | 1998-06-05 | 2000-07-04 | Protein Technologies International, Inc. | Recovery of isoflavones from soy molasses |
| CN101063158A (en) * | 2007-05-18 | 2007-10-31 | 东北农业大学 | Method for preparing soybean isoflavone aglycone |
| CN101824019A (en) * | 2009-12-17 | 2010-09-08 | 山东万得福实业集团有限公司 | Method for extracting isoflavone from soyabean molasses |
| CN103342691A (en) * | 2013-07-09 | 2013-10-09 | 内蒙古科然生物高新技术有限责任公司 | Method and equipment for extracting isoflavone, saponin and oligosaccharide from soy molasses |
Non-Patent Citations (3)
| Title |
|---|
| 张倩瑶: "大豆糖蜜分离提取异黄酮和皂甙的研究", 《江南大学硕士学位论文》 * |
| 彭游，等: "大豆异黄酮提取研究最新进展", 《大豆科学》 * |
| 石彦国，等: "不同大孔树脂对大豆糖蜜中异黄酮吸附影响研究", 《大豆科技》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108203445A (en) * | 2017-11-20 | 2018-06-26 | 荆门市德爱生物工程股份有限公司 | A kind of method using soy molasses production soybean lecithin |
| CN108203445B (en) * | 2017-11-20 | 2019-10-18 | 荆门市德爱生物工程股份有限公司 | A method of soybean lecithin is produced using soy molasses |
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| CN103965154B (en) | 2015-10-14 |
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Granted publication date: 20151014 |