CN105061382A - Method for synchronously extracting proanthocyanidin and selenium-enriched protein from black peanut skin - Google Patents
Method for synchronously extracting proanthocyanidin and selenium-enriched protein from black peanut skin Download PDFInfo
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- CN105061382A CN105061382A CN201510489469.0A CN201510489469A CN105061382A CN 105061382 A CN105061382 A CN 105061382A CN 201510489469 A CN201510489469 A CN 201510489469A CN 105061382 A CN105061382 A CN 105061382A
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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
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/14—Extraction; Separation; Purification
- C07K1/16—Extraction; Separation; Purification by chromatography
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/14—Extraction; Separation; Purification
- C07K1/30—Extraction; Separation; Purification by precipitation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/14—Extraction; Separation; Purification
- C07K1/36—Extraction; Separation; Purification by a combination of two or more processes of different types
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Abstract
The invention discloses a method for synchronously extracting proanthocyanidin and selenium-enriched protein from black peanut skin. Firstly, the black peanut skin subjected to liquid nitrogen freezing superfine grinding, then ultrasonic-assisted extraction of the proanthocyanidin and ultrasonic-assisted extraction of the selenium-enriched protein are performed simultaneously, prepared proanthocyanidin powder is high in proanthocyanidin content and high in activity, and the selenium-enriched protein is high in organic selenium content and high in activity. With the adoption of the method for preparing two active substances (the proanthocyanidin and the selenium-enriched protein) from the raw material, namely, the black peanut skin, the technological process can be simplified, the raw material cost can be reduced, the working efficiency can be improved, in addition, the method is high in extraction rate and suitable for industrial production, and the activity of extracted substances is high.
Description
Technical field
The present invention relates to a kind of blackcurrant pigment clothing proanthocyanidin and selenium-enriched protein synchronous extraction method, belong to peanut processing byproduct recycling field.
Background technology
The peanut of blackcurrant pigment to be underwear be black, its underwear color is pitch-black bright, and other parts are as Pericarppium arachidis hypogaeae, and Semen arachidis hypogaeae is then as good as with common peanut.Blackcurrant pigment is in the news rich in nutrition content, and compared with common peanut, containing more amino acid, be rich in selenium element, protein content is high, and output is high, and disease resistance is strong, therefore the dark favorable comment by plantation family and user, and cultivated area increases year by year.According to related documents, blackcurrant pigment has strong kidney and is healthy and strong, and in purged body, unnecessary lipid, anti-oxidant, and the effect such as delay senility, and its main functionally active material all exists with Testa arachidis hypogaeae.Have a lot of blackcurrant pigment goods at present, as blackcurrant pigment oil, peanut butter etc., need to remove Testa arachidis hypogaeae in the course of processing, these Testa arachidis hypogaeaes use as feed at present, and utilization ratio is low; Blackcurrant pigment clothing, mainly containing abundant nutritive substance, containing protein and the fat of about 17%, also contains natural active matter proanthocyanidin and organoselenium simultaneously.
Proanthocyanidin (proanthocyanidins) is the large class polyphenolic compound extensively existed in vegitabilia, is the general name of flavan-3-alcohol derivative.Be polymerized by catechin, l-Epicatechol, comprise dimer, tripolymer, the tetramer until ten aggressiveness.Proanthocyanidin has very strong biological activity, superfluous free radical in human body can be removed, and there is stronger resistance of oxidation, can be used as the principle active component of anti-cancer, anti-mutation and prevention and cure of cardiovascular disease medicine, can be used as the new type natural antioxidant of safety non-toxic.
Selenium is the necessary trace element of human body, which forms many active proteins, comprise Selenoperoxidase, it can protect body not by the infringement of the oxidative damage caused by free radical, in addition, there are some researches prove, selenium has the effect of inhibition thrombosis, it can also regulate the high-density in blood, the ratio of low density lipoprotein cholesterol, according to bibliographical information, selenium deficiency can cause heart trouble, the disorder of amyotrophy and function of human body, these situations are present in the middle of some animal species too, can clearly draw thus, be important by dietary int ake selenium be also necessary.In China, except the minority area such as Taiwan and enshi, the overwhelming majority is all in poor selenium area, therefore mend selenium raising our people body constitution is seemed particularly important, the form that organoselenium exists in vivo mainly contains seleno-protein, selenium polysaccharide and seleno nucleic acid etc., by food approach strengthening selenium element, become one of study hotspot of current functional foodstuff, there are market outlook very widely.The existence form of selenium mainly seleno-protein in peanut, can well supplement the demand of body to selenium.
The current extraction for organoselenium in blackcurrant pigment clothing and utilization have no and studies have reported that, simultaneously to the research of natural product in blackcurrant pigment clothing, the Isolation and purification of current rarely seen report black peanut skin pigment is the Isolation and purification technology of one matter; And containing various active material, the only some materials of Isolation and purification in blackcurrant pigment clothing, cause the waste of raw material and the increase of production cost, be unfavorable for the development of peanut industry.
Summary of the invention
In order to improve utilization ratio and the economic worth of blackcurrant pigment clothing and solve the problems such as Testa arachidis hypogaeae extracting substance is single, the invention provides a kind of blackcurrant pigment clothing proanthocyanidin and selenium-enriched protein synchronous extraction method, for achieving the above object, the technical solution adopted in the present invention is: liquid nitrogen freezing micronizing blackcurrant pigment clothing, and microwave radiation exaraction seleno-protein, its step of ultrasonic-assisted extraction proanthocyanidin comprise:
(1) super-micro wall-broken pulverizing is carried out after blackcurrant pigment clothing liquid nitrogen freezing 10min;
(2) the blackcurrant pigment clothing of pulverizing is added certain density ethanolic soln according to a certain percentage, put into Microwave Extraction Apparatus and carry out microwave auxiliary extraction;
(3) filter after extraction, filtrate is proanthocyanidin extracting solution; Filtrate is spray-dired blackcurrant pigment clothing proanthocyanidin after vacuum concentration;
(4) filter residue adds the alkaline solution of certain pH, and after stirring, supersound process certain hour, centrifugal at a certain temperature, and supernatant liquor regulates pH to iso-electric point.Leave standstill 10min, centrifugation, precipitates through column chromatography desalting treatment, collects protein liquid spraying dry and obtains selenium-enriched protein.
Preferably, a kind of blackcurrant pigment clothing proanthocyanidin and the blackcurrant pigment clothing micronizing described in selenium-enriched protein synchronous extraction method step (2), grinding particle size should at 5-10 μm; Testa arachidis hypogaeae powder after pulverizing is added the ethanolic soln of 50-70% in 1:2-1:5 ratio, in Microwave synthesize/catalysis instrument, carry out microwave extracting, extraction conditions is microwave power is 350-550w, and microwave temperature is 40-50 DEG C, and the microwave time is 2-6min.
Preferably, a kind of blackcurrant pigment clothing proanthocyanidin and the proanthocyanidin extracting solution spray drying condition described in selenium-enriched protein synchronous extraction method step (3) are pan feeding temperature is 40 DEG C, and inlet temperature is 160-180 DEG C, and air output is 22-25m
3/ h, obtains blackcurrant pigment clothing proanthocyanidin powder after drying completes.
Preferably, a kind of blackcurrant pigment clothing proanthocyanidin and the filter residue described in selenium-enriched protein synchronous extraction method step (4) add in the ratio of 1:2-1:4 the alkaline solution that pH is 8-9, at 50-60 DEG C, and supersound process 6-12min, centrifugal, supernatant liquor is regulated pH to 4-5, and centrifugation after standing 10min, precipitates through G-25 column chromatography desalting treatment, collect protein liquid spraying dry, drying conditions is pan feeding temperature is 50 DEG C, and inlet temperature is 180-190 DEG C, and air output is 25-27m
3/ h, obtains egg rich in selenium white powder after drying completes.
Beneficial effect of the present invention
(1) the present invention has carried out liquid nitrogen process ultra micro for pulverizing to Testa arachidis hypogaeae, can destroy the plant cell wall of Testa arachidis hypogaeae, be conducive to the stripping of extracting substance, can significantly improve extraction yield.
(2) the invention provides a kind of selenium-enriched protein and proanthocyanidin simultaneous extraction way, a technique prepares two kinds of materials, can improve the utilization ratio of Testa arachidis hypogaeae, avoid the waste of raw material, reduces production cost, improves the profit of processing enterprise.
(3) the present invention adopts the method for microwave-assisted, the Extracting temperature of reduction when preparing selenium-enriched protein, reduces leaching process to the destruction of organoselenium, improves the content of selenium in selenium-enriched protein; Shorten extraction time simultaneously, improve production efficiency.
(4) the present invention adopts the method for ultrasonic-assisted extraction when preparing proanthocyanidin, shortens extraction time, reduces Extracting temperature, and the proanthocyanidin anti-oxidant activity prepared is high, and extraction yield is high.
(5) the proanthocyanidin content prepared of the present invention is high, and active strong, can apply is in medicine, foods and cosmetics; The selenium-enriched protein organic selenium content of preparation is high, can meet the consumers demand of scarce selenium crowd, can be widely used in food and medicine.
Embodiment
Embodiment 1
Super-micro wall-broken pulverizing is carried out by after 100g blackcurrant pigment clothing liquid nitrogen freezing 10min; Testa arachidis hypogaeae after pulverizing should be added the ethanol of 70% of 200ml by grinding particle size below 10 μm, and in Microwave synthesize/catalysis instrument, carry out microwave extracting, extraction conditions is microwave power is 350w, and microwave temperature is 40 DEG C, and the microwave time is 6min.Filter after extraction, filtrate carries out spraying dry after vacuum concentration, and spray drying condition is pan feeding temperature is 40 DEG C, and inlet temperature is 160 DEG C, and air output is 25m
3/ h, obtains blackcurrant pigment clothing proanthocyanidin powder after drying completes.Filter residue adds the alkaline solution 200ml that pH is 8, and after stirring, supersound process 6min at 60 DEG C, the time, supernatant liquor regulates pH to 4.Leave standstill 10min, centrifugation, precipitates through column chromatography G-25 desalting treatment, and collect protein liquid and carry out spraying dry, drying conditions is pan feeding temperature is 50 DEG C, and inlet temperature is 180 DEG C, and air output is 25-27m
3/ h, obtains egg rich in selenium white powder after drying completes.After testing, the content of blackcurrant pigment clothing proanthocyanidin is 71%, and yield is 13%.In selenium-enriched protein, selenium content is 450ug/g, protein content 70%.
Controlled trial: ethanol 100g blackcurrant pigment clothing being added 70% of 200ml, carries out microwave extracting in Microwave synthesize/catalysis instrument, and extraction conditions is microwave power is 350w, and microwave temperature is 40 DEG C, and the microwave time is 6min.Filter after extraction, filtrate carries out spraying dry after vacuum concentration, and spray drying condition is pan feeding temperature is 40 DEG C, and inlet temperature is 160 DEG C, and air output is 25m
3/ h, obtains blackcurrant pigment clothing proanthocyanidin powder after drying completes.Filter residue adds the alkaline solution 200ml that pH is 8, and after stirring, supersound process 6min at 60 DEG C, the time, supernatant liquor regulates pH to 4.Leave standstill 10min, centrifugation, precipitates through column chromatography G-25 desalting treatment, and collect protein liquid and carry out spraying dry, drying conditions is pan feeding temperature is 50 DEG C, and inlet temperature is 180 DEG C, and air output is 25m
3/ h, obtains egg rich in selenium white powder after drying completes.After testing, the content of blackcurrant pigment clothing proanthocyanidin is 61%, and yield is 10%.In selenium-enriched protein, selenium content is 250ug/g, protein content 62%.
Embodiment 2
Super-micro wall-broken pulverizing is carried out by after 100g blackcurrant pigment clothing liquid nitrogen freezing 10min; Testa arachidis hypogaeae after pulverizing should be added the ethanol of 60% of 300ml by grinding particle size below 10 μm, and in Microwave synthesize/catalysis instrument, carry out microwave extracting, extraction conditions is microwave power is 450w, and microwave temperature is 45 DEG C, and the microwave time is 4min.Filter after extraction, filtrate carries out spraying dry after vacuum concentration, and spray drying condition is pan feeding temperature is 40 DEG C, and inlet temperature is 170 DEG C, and air output is 23m
3/ h, obtains blackcurrant pigment clothing proanthocyanidin powder (1) after drying completes.Filter residue adds the alkaline solution 300ml that pH is 8.5, and after stirring, supersound process 12min at 50 DEG C, the time, supernatant liquor regulates pH to 4.5.Leave standstill 10min, centrifugation, precipitates through column chromatography G-25 desalting treatment, and collect protein liquid and carry out spraying dry, drying conditions is pan feeding temperature is 50 DEG C, and inlet temperature is 190 DEG C, and air output is 26m
3/ h, obtains egg rich in selenium white powder (1) after drying completes.After testing, the content of blackcurrant pigment clothing proanthocyanidin powder (1) Procyanidins is 73%, and yield is 14%.In selenium-enriched protein, selenium content is 550ug/g, protein content 72%.
Controlled trial
Super-micro wall-broken pulverizing is carried out by after 100g blackcurrant pigment clothing liquid nitrogen freezing 10min; The ethanol that Testa arachidis hypogaeae after pulverizing should be added 60% of 300ml by grinding particle size below 10 μm extracts 20min at temperature is 55 DEG C.Filter after extraction, filtrate carries out spraying dry after vacuum concentration, and spray drying condition is pan feeding temperature is 40 DEG C, and inlet temperature is 170 DEG C, and air output is 23m
3/ h, obtains blackcurrant pigment clothing proanthocyanidin powder (2) after drying completes.Filter residue adds the alkaline solution 300ml that pH is 8.5, after stirring, at 60 DEG C, extracts 30min, centrifugal, and supernatant liquor regulates pH to 4.5.Leave standstill 10min, centrifugation, precipitates through column chromatography G-25 desalting treatment, and collect protein liquid and carry out spraying dry, drying conditions is pan feeding temperature is 50 DEG C, and inlet temperature is 190 DEG C, and air output is 26m
3/ h, obtains egg rich in selenium white powder (2) after drying completes.After testing, the content of blackcurrant pigment clothing proanthocyanidin powder Procyanidins (2) is 59%, and yield is 11%.In selenium-enriched protein (2), selenium content is 350ug/g, protein content 62%.
Testa arachidis hypogaeae proanthocyanidin powder (1) resistance of oxidation is (2) 2.3 times, Testa arachidis hypogaeae proanthocyanidin powder, and selenium-enriched protein (1) resistance of oxidation is 1.6 times of selenium-enriched protein (2).
Embodiment 3
Super-micro wall-broken pulverizing is carried out by after 100g blackcurrant pigment clothing liquid nitrogen freezing 10min; Testa arachidis hypogaeae after pulverizing should be added the ethanol of 70% of 400ml by grinding particle size below 10 μm, and in Microwave synthesize/catalysis instrument, carry out microwave extracting, extraction conditions is microwave power is 550w, and microwave temperature is 50 DEG C, and the microwave time is 2min.Filter after extraction, filtrate carries out spraying dry after vacuum concentration, and spray drying condition is pan feeding temperature is 40 DEG C, and inlet temperature is 180 DEG C, and air output is 25m
3/ h, obtains blackcurrant pigment clothing proanthocyanidin powder after drying completes.Filter residue adds the alkaline solution 400ml that pH is 9, and after stirring, supersound process 12min at 40 DEG C, the time, supernatant liquor regulates pH to 5.Leave standstill 10min, centrifugation, precipitates through column chromatography G-25 desalting treatment, and collect protein liquid and carry out spraying dry, drying conditions is pan feeding temperature is 50 DEG C, and inlet temperature is 190 DEG C, and air output is 26m
3/ h, obtains egg rich in selenium white powder after drying completes.After testing, the content of blackcurrant pigment clothing proanthocyanidin powder Procyanidins is 75%, and yield is 13%.In selenium-enriched protein, selenium content is 650ug/g, protein content 75%.
The above, be only the specific embodiment of the present invention, is not limited thereto, and is anyly familiar with those skilled in the art in the technical scope that the present invention discloses, and can expect change easily or replace, all should be encompassed within protection scope of the present invention.
Claims (4)
1. blackcurrant pigment clothing proanthocyanidin and a selenium-enriched protein synchronous extraction method, its feature comprises the following steps:
(1) super-micro wall-broken pulverizing is carried out after blackcurrant pigment clothing liquid nitrogen freezing 10min;
(2) the blackcurrant pigment clothing of pulverizing is added certain density ethanolic soln according to a certain percentage, put into Microwave Extraction Apparatus and carry out microwave auxiliary extraction;
(3) filter after extraction, filtrate is proanthocyanidin extracting solution; Filtrate is spray-dired blackcurrant pigment clothing proanthocyanidin after vacuum concentration;
(4) filter residue adds the alkaline solution of certain pH, and after stirring, supersound process certain hour, centrifugal at a certain temperature, and supernatant liquor regulates pH to iso-electric point.Leave standstill 10min, centrifugation, precipitates through column chromatography desalting treatment, collects protein liquid spraying dry and obtains selenium-enriched protein.
2. a kind of blackcurrant pigment clothing proanthocyanidin according to claim 1 and selenium-enriched protein synchronous extraction method, is characterized in that, the blackcurrant pigment clothing micronizing described in step (1), and grinding particle size should at 5-10 μm; Testa arachidis hypogaeae powder after pulverizing is added the ethanolic soln of 50-70% in 1:2-1:5 ratio, in Microwave synthesize/catalysis instrument, carry out microwave extracting, extraction conditions is microwave power is 350-550w, and microwave temperature is 40-50 DEG C, and the microwave time is 2-6min.
3. a kind of blackcurrant pigment clothing proanthocyanidin according to claim 1 and selenium-enriched protein synchronous extraction method, it is characterized in that, proanthocyanidin extracting solution spray drying condition described in step (3) is pan feeding temperature is 40 DEG C, and inlet temperature is 160-180 DEG C, and air output is 22-25m
3/ h, obtains blackcurrant pigment clothing proanthocyanidin powder after drying completes.
4. a kind of blackcurrant pigment clothing proanthocyanidin according to claim 1 and selenium-enriched protein synchronous extraction method, it is characterized in that, filter residue described in step (4) adds in the ratio of 1:2-1:4 the alkaline solution that pH is 8-9, at 50-60 DEG C, supersound process 6-12min, centrifugal, supernatant liquor is regulated pH to 4-5, centrifugation after standing 10min, precipitation is through G-25 column chromatography desalting treatment, and collect protein liquid spraying dry, drying conditions is pan feeding temperature is 50 DEG C, inlet temperature is 180-190 DEG C, and air output is 25-27m
3/ h, obtains egg rich in selenium white powder after drying completes.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105614759A (en) * | 2015-12-29 | 2016-06-01 | 山东美佳集团有限公司 | Preparation method of nano-selenium mussel powder |
| CN106053741A (en) * | 2016-08-09 | 2016-10-26 | 孙杰 | Quality determination method of black peanuts for pigment extraction and evaluation method thereof |
| CN108741058A (en) * | 2018-06-14 | 2018-11-06 | 陕西博硒农业科技股份有限公司 | A kind of selenium-rich food additive and preparation method and application |
| CN108936235A (en) * | 2018-06-14 | 2018-12-07 | 陕西博硒农业科技股份有限公司 | A kind of beautifying face and moistering lotion selenium-rich nutritive powder and preparation method thereof |
| CN109401358A (en) * | 2017-08-16 | 2019-03-01 | 冯顺珍 | A method of haematochrome is extracted from Jasmine flower residue |
| CN109400669A (en) * | 2018-12-06 | 2019-03-01 | 西南林业大学 | The small protein extracting method of walnut kernel skin and application |
-
2015
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| 吕晓玲: "黑花生衣色素的提取工艺条件研究", 《食品研究与开发》 * |
| 王锋等: "黑花生的主要品质性状及黑花生衣色素的提取工艺研究", 《中国食品添加剂》 * |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105614759A (en) * | 2015-12-29 | 2016-06-01 | 山东美佳集团有限公司 | Preparation method of nano-selenium mussel powder |
| CN106053741A (en) * | 2016-08-09 | 2016-10-26 | 孙杰 | Quality determination method of black peanuts for pigment extraction and evaluation method thereof |
| CN106053741B (en) * | 2016-08-09 | 2018-09-11 | 孙杰 | A kind of the quality determination method and its evaluation method of pigment extraction blackcurrant pigment |
| CN109401358A (en) * | 2017-08-16 | 2019-03-01 | 冯顺珍 | A method of haematochrome is extracted from Jasmine flower residue |
| CN108741058A (en) * | 2018-06-14 | 2018-11-06 | 陕西博硒农业科技股份有限公司 | A kind of selenium-rich food additive and preparation method and application |
| CN108936235A (en) * | 2018-06-14 | 2018-12-07 | 陕西博硒农业科技股份有限公司 | A kind of beautifying face and moistering lotion selenium-rich nutritive powder and preparation method thereof |
| CN109400669A (en) * | 2018-12-06 | 2019-03-01 | 西南林业大学 | The small protein extracting method of walnut kernel skin and application |
| CN109400669B (en) * | 2018-12-06 | 2021-08-20 | 西南林业大学 | Extraction method and application of micromolecular protein of walnut kernel peel |
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Effective date of registration: 20190305 Address after: 266600 No. 38 Zhifu Road, Wangcheng Street Office, Laixi City, Qingdao City, Shandong Province Patentee after: Shandong Peanut Inst. Address before: 266600 No. 38 Zhifu Road, Wangcheng Street Office, Laixi City, Qingdao City, Shandong Province Co-patentee before: Shandong Peanut Inst. Patentee before: Zhang Chushu |