CN103073914A - Method for extracting maize yellow pigment from maize protein - Google Patents
Method for extracting maize yellow pigment from maize protein Download PDFInfo
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Abstract
The invention relates to the technical field of corn gluten meal deep processing, in particular to a method for extracting maize yellow pigment from maize protein. The method comprises the following steps of performing superfine grinding on the corn gluten meal into ultra-fine powder of which the particle size is 300 to 500 meshes, adding water, xylanase and aspergillus oryzae protease into the ultra-fine powder to perform enzymolysis on the ultra-fine powder, centrifuging the enzymatic hydrolysate, and removing the supernate to obtain a precipitate; adding ethanol into the precipitate, extracting the mixture in a microwave reaction system, and collecting the supernate; and removing protein from the supernate, concentrating the filtrate under reduced pressure to obtain a paste, and freezing the paste under vacuum to dry the paste until the weight of the paste is consistent. The xylanase and the aspergillus oryzae protease are adopted to perform enzymolysis on the maize protein ultra-fine powder, so that the extraction rate of the maize yellow pigment is well improved; and the step of superfine grinding facilitates the dissolving of the maize yellow pigment in an extraction process.
Description
Technical field
The present invention relates to Zein powder deep process technology field, particularly from zein, extract the method for corn yellow OB.
Background technology
Corn yellow OB is the mixture of several Carotenoids, and wherein two hydroxyl carotene account for 81.2%, monohydroxy carotene 17.2%, and carotene is about 1.6%.Blessin in 1962 has confirmed that corn yellow OB exists with complex form in protein in corn.Its content is different because of corn kind and protein content, both at home and abroad in the report in the Zein powder content of corn yellow OB mostly between 300 μ g/g-700 μ g/g.Wherein a plurality of conjugated double bonds make it have strikingly color in the hydroxyl carotene, and xenthophylls is not the precursor of VA, even can not be converted after the intestinal absorption, can keep to greatest extent unique characteristics.Therefore at present domestic processing to Zein powder is mostly through adding as the fowl poultry kind feed nutrition after slightly carrying.
In recent years, the functional performance of corn yellow OB causes people's attention gradually, and the people's such as Slattery M L in 2000 research finds that often the edible food that is rich in carotenoid can reduce the danger of AMD; People's driven mechanics angle researchs such as Petra A Th ü rmann in 2005 have also explained that zeaxanthin and lutein act on effect and the mechanism of AMD; The people such as Jean Soon Park find in research in 1998, xenthophylls can suppress generation and the growth of breast tumor significantly, in addition, multinomial studies show that, corn yellow OB has restraining effect to kinds cancers such as mammary cancer, prostate cancer, skin carcinomas, and it is in that to suppress active oxygen radical research active and that slow down aspect the organ senescence also more and more deep.
As natural pigment, corn yellow OB is approved as food dye by many American-European countries, China food hygienic standard GB2760-1986 regulation, allow corn yellow OB as foodstuff additive, in addition, China's food security standard GB26405-2011 has stipulated the examination criteria of total carotinoid, xenthophylls and zeaxanthin in the foodstuff additive xenthophylls.
At present, the preparation method of corn yellow OB mainly contains usual vehicle lixiviate and new and high technology Assisted Extraction.As patent CN 00134539 disclosed adopt the ascending different solvents lixiviate of polarity, employing hexane and ethyl acetate that polarity is little, polarity general election propyl alcohol etc. also need processing with enzyme preparation after the extraction, the time is long, complicated operation; Disclosed such as patent CN 99106874, adopt supercritical extraction, though the higher apparatus expensive of purity be difficult to be applied to suitability for industrialized production, and extraction yield is low; Disclosed such as patent application 101280121, adopt microwave-ultrasonic to extract corn yellow OB, shortened extraction time, but the heat effect that High-Power Microwave causes makes the reactive system difficult control of temperature, unfavorable suitability for industrialized production, and the normal hexane wash-out may cause reluctant dissolvent residual problem, food-processing industry difficult the application.
In the prior art, the record of using enzymolysis process to extract other materials of acquisition from zein is arranged also, use mostly be proteolytic enzyme and cellulase, mainly be enzymolysis protein and Mierocrystalline cellulose wherein, to reach better extraction effect.
Summary of the invention
In order to solve the above complicated operation that from zein, extracts corn yellow OB, to be difficult to realize the problem of suitability for industrialized production, the invention provides high, the simple to operation method of from zein, extracting corn yellow OB of a kind of extraction yield.
The present invention is achieved by the following measures:
A kind of method of extracting corn yellow OB from zein may further comprise the steps:
(1) the Zein powder super-fine powder is broken into 300 orders to 500 purpose super-fine powder, add entry, the zytase and the aspergillus oryzae protease that accounts for enzyme activity 〉=60000IU/g of super-fine powder quality 0.3%-1.2% that add the enzyme activity 〉=15000IU/g that accounts for super-fine powder quality 0.1%-0.5%, the super-fine powder mass concentration is 3%-5%, enzymolysis 2-5h under 42 ± 5 ℃ of conditions, enzymolysis solution is centrifugal, abandons supernatant liquor, gets precipitation;
(2) add ethanol in the precipitation in the step (1), quality is extracted in the microwave reaction system for 12-18 times of precipitation, and microwave power is 220W-480W, time 85s-115s, and temperature is 42 ± 5 ℃, and is centrifugal, collects supernatant liquor;
(3) supernatant liquor filters in-18 ℃ of lower storage 10h, and filtrate is concentrated, obtains paste, is drying to obtain.
Described method, zytase account for super-fine powder quality 0.5%, and aspergillus oryzae protease accounts for super-fine powder quality 1.2%.
The ethanol volumetric concentration of using in the described method, step (2) is 95%, and quality is 15 times of precipitation.
Described method is filtered into room temperature and descended low speed filter paper decompress filter, to remove the protein that is cotton-shaped in the step (3).
Filtrate simmer down to concentrating under reduced pressure in the described method, step (3).
Drying is vacuum lyophilization in the described method, step (3).
Described method, centrifugal in the step (2) is with 10000r/min rotating speed high speed centrifugation 10min.
The inventive method is extracted in the corn yellow OB process, solvent for use only is ethanol, avoided the residue problem of other low toxicity or easy intoxicating solvent, and ethanol can be changed to foodstuffs industry 90%-95% ethanol commonly used, products therefrom namely can be used as the raw materials for production of foodstuff additive or functional foodstuff, is beneficial to suitability for industrialized production.
Beneficial effect of the present invention:
1, method of the present invention uses zytase and aspergillus oryzae protease that the zein super-fine powder is carried out enzymolysis, to improving the corn yellow OB extraction yield good promoter action is arranged;
2, thereby micronizing greatly reduces raw material granularity and increases and the extraction solvent contact area, and simultaneously crushing process Ester structural damage effect that the destruction of cell and enzymolysis processing are composited to protein and corn yellow OB is conducive to the stripping of corn yellow OB in the leaching process more;
3, solvent is single, can directly replace with food grade ethanol, produces foodstuff additive and functional food, the potential danger factors such as no solvent residue;
4, the low-temperature microwave Assisted Extraction shortens extraction time greatly;
5, technique is simple, is easy to industrialization and transforms.
Embodiment
For a better understanding of the present invention, further specify below in conjunction with specific embodiment.Raw material
Embodiment 1:
(1) the Zein powder super-fine powder is broken into 300 purpose super-fine powder, take by weighing 2g zein super-fine powder in reaction unit, add deionized water, control super-fine powder mass concentration is 4%, adding the enzyme activity that accounts for super-fine powder quality 0.3% is that the zytase of 15000IU/g and the enzyme activity that accounts for super-fine powder quality 0.8% are the aspergillus oryzae protease of 60000IU/g, enzymolysis 4h under 42 ± 5 ℃ of conditions, and enzymolysis solution is centrifugal, abandon supernatant liquor, get precipitation;
(2) add ethanol in the precipitation in the step (1), press the ethanol that solid-liquid ratio 1:12 adds 24mL90%, in the microwave reaction system, extract, microwave power is 220W, time 115s, and temperature is 42 ± 5 ℃, react complete, with 10000r/min rotating speed high speed centrifugation 10min, collect supernatant liquor;
(3) supernatant liquor is in-18 ℃ of lower storage 10h, and room temperature was descended low speed filter paper decompress filter, removed the protein that is cotton-shaped; Filtrate decompression is concentrated, obtains paste, and vacuum lyophilization is to constant weight, and get final product.
Calculating extraction yield is 5.82%.
Embodiment 2:
(1) the Zein powder super-fine powder is broken into 500 purpose super-fine powder, take by weighing 2g zein super-fine powder in reaction unit, add deionized water, control super-fine powder mass concentration is 5%, adding the enzyme activity that accounts for super-fine powder quality 0.5% is that the zytase of 15000IU/g and the enzyme activity that accounts for super-fine powder quality 1.2% are the aspergillus oryzae protease of 60000IU/g, enzymolysis 5h under 42 ± 5 ℃ of conditions, and enzymolysis solution is centrifugal, abandon supernatant liquor, get precipitation;
(2) add ethanol in the precipitation in the step (1), press the ethanol that solid-liquid ratio 1:15 adds 30mL95%, in the microwave reaction system, extract, microwave power is 480W, time 115s, and temperature is 42 ± 5 ℃, react complete, with 10000r/min rotating speed high speed centrifugation 10min, collect supernatant liquor;
(3) supernatant liquor is in-18 ℃ of lower storage 10h, and room temperature was descended low speed filter paper decompress filter, removed the protein that is cotton-shaped; Filtrate decompression is concentrated, obtains paste, and vacuum lyophilization is to constant weight, and get final product.
Calculating extraction yield is 6.53%.
Embodiment 3:
(1) the Zein powder super-fine powder is broken into 400 purpose super-fine powder, take by weighing 2g zein super-fine powder in reaction unit, add deionized water, control super-fine powder mass concentration is 3%, adding the enzyme activity that accounts for super-fine powder quality 0.1% is that the zytase of 15000IU/g and the enzyme activity that accounts for super-fine powder quality 0.3% are the aspergillus oryzae protease of 60000IU/g, enzymolysis 2h under 42 ± 5 ℃ of conditions, and enzymolysis solution is centrifugal, abandon supernatant liquor, get precipitation;
(2) add ethanol in the precipitation in the step (1), press the ethanol that solid-liquid ratio 1:18 adds 36mL92%, in the microwave reaction system, extract, microwave power is 360W, time 85s, and temperature is 42 ± 5 ℃, react complete, with 10000r/min rotating speed high speed centrifugation 10min, collect supernatant liquor;
(3) supernatant liquor is in-18 ℃ of lower storage 10h, and room temperature was descended low speed filter paper decompress filter, removed the protein that is cotton-shaped; Filtrate decompression is concentrated, obtains paste, and vacuum lyophilization is to constant weight, and get final product.
Calculating extraction yield is 5.69%.
Embodiment 4:
(1) the Zein powder super-fine powder is broken into 500 purpose super-fine powder, take by weighing 2g zein super-fine powder in reaction unit, add deionized water, control super-fine powder mass concentration is 5%, adding the enzyme activity that accounts for super-fine powder quality 0.5% is the zytase of 15000IU/g, enzymolysis 5h under 42 ± 5 ℃ of conditions, and enzymolysis solution is centrifugal, abandon supernatant liquor, get precipitation;
(2) add ethanol in the precipitation in the step (1), press the ethanol that solid-liquid ratio 1:15 adds 30mL95%, in the microwave reaction system, extract, microwave power is 480W, time 115s, and temperature is 42 ± 5 ℃, react complete, with 10000r/min rotating speed high speed centrifugation 10min, collect supernatant liquor;
(3) supernatant liquor is in-18 ℃ of lower storage 10h, and room temperature was descended low speed filter paper decompress filter, removed the protein that is cotton-shaped; Filtrate decompression is concentrated, obtains paste, and vacuum lyophilization is to constant weight, and get final product.
Calculating extraction yield is 4.77%.
Embodiment 5:
(1) the Zein powder super-fine powder is broken into 500 purpose super-fine powder, take by weighing 2g zein super-fine powder in reaction unit, add deionized water, control super-fine powder mass concentration is 5%, adding the enzyme activity that accounts for super-fine powder quality 1.2% is the aspergillus oryzae protease of 60000IU/g, enzymolysis 5h under 42 ± 5 ℃ of conditions, and enzymolysis solution is centrifugal, abandon supernatant liquor, get precipitation;
(2) add ethanol in the precipitation in the step (1), press the ethanol that solid-liquid ratio 1:15 adds 30mL95%, in the microwave reaction system, extract, microwave power is 480W, time 115s, and temperature is 42 ± 5 ℃, react complete, with 10000r/min rotating speed high speed centrifugation 10min, collect supernatant liquor;
(3) supernatant liquor is in-18 ℃ of lower storage 10h, and room temperature was descended low speed filter paper decompress filter, removed the protein that is cotton-shaped; Filtrate decompression is concentrated, obtains paste, and vacuum lyophilization is to constant weight, and get final product.
Calculating extraction yield is 4.58%.
Embodiment 6:
(1) Zein powder that will process without micronizing (crossing approximately 20 orders-40 order sample sifter), take by weighing 2g zein super-fine powder in reaction unit, add deionized water, control super-fine powder mass concentration is 5%, adding the enzyme activity that accounts for super-fine powder quality 0.5% is that the zytase of 15000IU/g and the enzyme activity that accounts for super-fine powder quality 1.2% are the aspergillus oryzae protease of 60000IU/g, enzymolysis 5h under 42 ± 5 ℃ of conditions, and enzymolysis solution is centrifugal, abandon supernatant liquor, get precipitation;
(2) add ethanol in the precipitation in the step (1), press the ethanol that solid-liquid ratio 1:15 adds 30mL95%, in the microwave reaction system, extract, microwave power is 480W, time 115s, and temperature is 42 ± 5 ℃, react complete, with 10000r/min rotating speed high speed centrifugation 10min, collect supernatant liquor;
(3) supernatant liquor is in-18 ℃ of lower storage 10h, and room temperature was descended low speed filter paper decompress filter, removed the protein that is cotton-shaped; Filtrate decompression is concentrated, obtains paste, and vacuum lyophilization is to constant weight, and get final product.
Calculating extraction yield is 4.32%.
Claims (7)
1. method of extracting corn yellow OB from zein is characterized in that may further comprise the steps:
(1) the Zein powder super-fine powder is broken into 300 orders to 500 purpose super-fine powder, add entry, the zytase and the aspergillus oryzae protease that accounts for enzyme activity 〉=60000IU/g of super-fine powder quality 0.3%-1.2% that add the enzyme activity 〉=15000IU/g that accounts for super-fine powder quality 0.1%-0.5%, the super-fine powder mass concentration is 3%-5%, enzymolysis 2-5h under 42 ± 5 ℃ of conditions, enzymolysis solution is centrifugal, abandons supernatant liquor, gets precipitation;
(2) add ethanol in the precipitation in the step (1), quality is extracted in the microwave reaction system for 12-18 times of precipitation, and microwave power is 220W-480W, time 85s-115s, and temperature is 42 ± 5 ℃, and is centrifugal, collects supernatant liquor;
(3) supernatant liquor filters in-18 ℃ of lower storage 10h, and filtrate is concentrated, obtains paste, is drying to obtain.
2. method according to claim 1 is characterized in that zytase accounts for super-fine powder quality 0.5%, and aspergillus oryzae protease accounts for super-fine powder quality 1.2%.
3. method according to claim 1 and 2 is characterized in that the ethanol volumetric concentration of using in the step (2) is 95%, and quality is 15 times of precipitation.
4. method according to claim 1 and 2 is characterized in that being filtered in the step (3) room temperature and descended low speed filter paper decompress filter, to remove the protein that is cotton-shaped.
5. method according to claim 1 and 2 is characterized in that filtrate simmer down to concentrating under reduced pressure in the step (3).
6. method according to claim 1 and 2 is characterized in that dry in the step (3) is vacuum lyophilization.
7. method according to claim 1 and 2 is characterized in that centrifugal in the step (2) is with 10000r/min rotating speed high speed centrifugation 10min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105647231A (en) * | 2016-03-25 | 2016-06-08 | 贵州大学 | Process for extracting curcumine in enzymic method-microwave method combination way |
| CN107897646A (en) * | 2017-11-21 | 2018-04-13 | 成都新柯力化工科技有限公司 | A kind of method using laser assisted extraction corn yellow OB food additives |
| CN109082911A (en) * | 2018-07-05 | 2018-12-25 | 佛山市衣香蒂丝服装设计有限公司 | A kind of colouring method of dye yam extracting solution to silk fabric |
| CN110241165A (en) * | 2019-07-03 | 2019-09-17 | 齐鲁工业大学 | A method of luteole is extracted from corn protein powder enzymatic hydrolysis jelly |
| CN111575263A (en) * | 2020-05-12 | 2020-08-25 | 武汉新华扬生物股份有限公司 | Complex enzyme preparation for extracting zeaxanthin and extraction method |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110256319B (en) * | 2019-07-03 | 2021-01-05 | 齐鲁工业大学 | Method for extracting zeaxanthin from enzymolysis corn protein powder |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109082911A (en) * | 2018-07-05 | 2018-12-25 | 佛山市衣香蒂丝服装设计有限公司 | A kind of colouring method of dye yam extracting solution to silk fabric |
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| CN110241165B (en) * | 2019-07-03 | 2021-05-18 | 齐鲁工业大学 | Method for extracting zeaxanthin from corn gluten meal enzymolysis jelly |
| CN111575263A (en) * | 2020-05-12 | 2020-08-25 | 武汉新华扬生物股份有限公司 | Complex enzyme preparation for extracting zeaxanthin and extraction method |
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