CN1952094A - Process for extracting sunflower seed oil and recovering protein by aqueous enzymatic method - Google Patents
Process for extracting sunflower seed oil and recovering protein by aqueous enzymatic method Download PDFInfo
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Abstract
The method relates to the method to extract the sunflower oil and recover the protein by water-enzyme method. The producing procedure comprises the following steps: dry-pulverizing the uncoated sunflower seed, adding citrate buffer to the powder and decomposing the powder by compound cellulose; centrifugalizing to get free oil, emulsion, digest and tablet; high speed centrifugalizing to get some free oil; filtering, vacuum concentrating, alcohol precipitating, centrifugalizing and freeze-drying to recycle the protein. The special treatment in the invention has substantially increased the free oil yield and the quality of the free oil is better than the refined oil. The water-extracting and alcohol-precipitating method to get the protein is simple and efficient; besides, the method has maintained the sunflower protein's nutritive value and functional value very well. Compared with the traditional squeezing and water-extracting technologies, the invention has many advantages such as simple producing equipments, safe operation, less energy expenditure and less pollution.
Description
Technical field
A kind of aqueous enzymatic extraction sunflower seed oil and reclaim method of protein belongs to the technical field of aqueous enzymatic method oil extracting process.
Background technology
Contain grease in the polly seed nucleole more than 50%, wherein contain abundant indispensable fatty acid, linoleic acid content is up to 66%, and oleic acid content is about 15%.High-load linoleic plus oleic acid makes sunflower seed oil have the characteristic above other plant oil dissolving cholesterol ability, therefore long-term edible sunflower seed oil, the function that reduces cholesterol in human body content is arranged, help the control of cardiovascular diseases and hyperlipidemia, reach the effect that strengthens HUMAN HEALTH and promote longevity, so sunflower seed oil leaps to the hat of edible oil with its unique health protection effect.Sunflower seed oil after the refining is limpid faint yellow or bluish yellow look, its smell fragrance, and flavour is pure, and the ratio of linoleic acid content and content of vitamin E is balanced, is convenient to the absorption of human body utilization, and the human consumption rate reaches 96.5%.So sunflower seed oil is the good edible oil that nutritive value is very high, be of value to HUMAN HEALTH, it has become the senior edible vegetable oil of generally acknowledging in the world at present.
Contain protein 21 %～31% in the sunflower benevolence, wherein, sphaeroprotein accounts for 55～60%, and protamine accounts for 17～23%, and gluten accounts for 11～17%, and prolamine accounts for 1～4%.Sunflower seeds only is used for oil expression usually, makes pot foods and oil plant food, its albumen and carbohydrate are underutilized, along with the exploitation to new egg-white food, people recognize to contain in the sunflower seeds and are higher than other cereal quality proteins, are one of important sources of vegetable-protein in recent years.Sunflower protein not only has water-absorbent, oil absorbency, emulsifying property and spumescence preferably, also has higher nutritive value, in the sunflower protein except lysine content is low, other indispensable amino acid all is higher than or pushes away (FAO) value of building with Food and Argriculture OrganizationFAO and conforms to, and has good balance.Do not have toxic ingredient or anti-nutritional factors in the sunflower seeds, chlorogenic acid is the main phenolic compound that influences the sunflower protein quality.When extracting protein under neutrality and alkaline condition, because the effect of polyphenoloxidase or atmospheric oxygen, chlorogenic acid is easy to be oxidized to green quinone, makes the albumen variable color.The green product that chlorogenic acid generates not only influences proteinic color, and chlorogenic acid can suppress stomach en-, therefore must be removed in extracting protein process, to guarantee quality product.
At present, the mechanize oil plant complete processing that adopted of Semen Helianthi system oil is to produce from the heavy handicraft workshop of five sixties of last century oil plant processing and semi-mechanization progressively to grow up.The sunflower seeds oil-producing technique process of China is: shelling, pre-press for extracting juice, leaching.Milling process can keep the flavour of product, but this method residual oil content height, labour intensity is big, cost is high, power consumption is big, and protein denaturation is serious in the grouts, can only be used as fertilizer, causes the proteic waste of a large amount of quality plants.Sunflower seeds lixiviation process oil-producing technique and equipment are processed identical with soybean, vegetable seed.Lixiviation process production efficiency height and residual oil content is low, but its required equipment is many, the investment big; The crude oil complicated component needs strict refining treatment, and the oil product flavor loss is big; Wet dregs of rice sex change in high temperature precipitation process is big; With an organic solvent increased technology loaded down with trivial details property, reduced the security of producing, the pollution that has caused environment; Micro-organic solvent residual in the processed oil has harm to human health.
Aqueous enzymatic method is carried the oil tech of carrying that oil is a kind of novelty, safer reliable, reported once that the enzyme that uses had cellulase, hemicellulase, polygalacturonase, amylase and proteolytic enzyme etc., prozyme has the activity of plurality of enzymes, produced synergy for cell wall breaking, particularly effective.Nineteen eighty-three Fullbrook has been applied to aqueous enzymatic method the extraction of soybean and rapeseed oil.For some seeds, as: vegetable seed, and fruit, as coconut, olive, the optimizing condition that aqueous enzymatic method is carried oil all has report.People such as J.Sineiro in 1997 have utilized aqueous enzymatic extraction sunflower seed oil, though oil extracting rate is not high, its result helps to screen more effective enzyme.China adopts the research report of aqueous enzymatic extraction plant seed oil later, from Wang Zhang in 1994, professor Xu Shiying at home reported first since the aqueous enzymatic extraction soybean oil, this The Application of Technology only limits to materials such as soybean, maize germ, vegetable seed and peanut.
Contain chlorogenic acid, oligose, albumen and pectin etc. in the hydrolyzed solution that centrifugation goes out after the aqueous enzymatic extraction sunflower seed oil.Owing to temperature, salting in effect and albumen and fat combine reason such as formation lipoprotein etc., make that most of protein is present in wherein in the raw material.The research of directly reclaiming sunflower protein at present from hydrolyzed solution yet there are no other report.Reclaiming this part albumen must remove the chlorogenic acid that is dissolved in the hydrolyzed solution, avoids it to influence protein quality.Use separable sunflower protein of water extraction and alcohol precipitation method and chlorogenic acid, shortcoming is to make protein denaturation, can effectively control by reducing method of temperature.
Summary of the invention
The purpose of this invention is to provide a kind of aqueous enzymatic extraction sunflower seed oil and reclaim method of protein.On the basis of determining enzyme process oil extracting process route, obtain higher free oil yield by optimizing technology, reclaim the protein in the hydrolyzed solution simultaneously.
Technical scheme of the present invention: the shelling sunflower seeds is after dry ground, add citrate buffer, carry out enzyme digestion reaction with complex cellulase, it is centrifugal that enzymolysis finishes the back, obtain free oil, milk sap, hydrolyzed solution and grouts, the milk sap that obtains is through high speed centrifugation, and the part of reentrying free oil, hydrolyzed solution are after filtration, vacuum concentration, alcohol precipitation, centrifugal, precipitation and lyophilize reclaim and obtain protein.
1. operational path, as shown in Figure 1.
2. analytical procedure
The mensuration of moisture content: atmosphere pressure desiccation
The mensuration of fat content: soxhlet extraction
The mensuration of protein content: micro-Kjeldahl determination
The mensuration of total ash content: dry ashing method
The mensuration of crude fiber content: weighting method
The mensuration of carbohydrate content: direct titrimetric method
The mensuration of reducing sugar content: DNS method
The mensuration of chlorogenic acid content: ultraviolet spectrophotometry
3. processing condition
Dry ground: promptly pulverize the shelling sunflower seeds with medicinal herb grinder, destroy the histocyte of raw material, degree of grinding is high more, the area that enzyme can act on is just big more, oil extracting rate also can improve accordingly, but degree of grinding is too high, and fat, protein significantly discharge, emulsion is serious, and oil extracting rate is had bigger influence.
Enzymolysis process: the shelling sunflower seeds after the pulverizing is by 3: 1-7: the liquid of 1 (w/w)/seed is than the 0.05mol/L citrate buffer that adds pH4.8, stir evenly the complex cellulase that adds after the form slurry in shelling sunflower seeds quality 1%-3%, temperature in the enzymolysis process is 50 ℃, stirring velocity is 250r/min, enzymolysis 5-7h.Enzymolysis solution is directly centrifugal, and centrifugal speed is 3000r/min, separates to obtain free oil I, emulsus liquid layer I, hydrolyzed solution and grouts.The emulsus liquid layer I that obtains is carried out again centrifugal, centrifugal force is 8000g, separates to obtain free oil II and emulsus liquid layer II.Under preferred processing condition, merge free oil I and free oil II, total free oil yield can reach 85%-90%.
Plant cell wall mainly is made up of Mierocrystalline cellulose and polysaccharose substance, and protein is wrapped in wherein by cellulose substances.Utilize the cellulose skeleton of complex cellulase degradable plant cell walls, make cell wall breaking and collapse, effective constituent dissociates out in the cell, improves the yield of free oil.The used complex cellulase of the present invention is the Viscozyme L of NOVO company.
In the system that the protein of oil-containing, water and tool amphipathic characteristic exists, can form milk sap inevitably in the whipping process.Accelerate stirring velocity, can destroy the formation of milk sap, reduce the milk sap volume, improve the free oil yield.
The hydrolyzed solution that obtains after centrifugal is used to reclaim protein, and water lotion that the washing grouts obtain and the merging of this hydrolyzed solution can further improve protein recovery.
Reclaim protein: after hydrolyzed solution filtered, vacuum concentration was the ethanol sedimentation of 50%-75% to the solid content of 9%-15% with-20 ℃ final concentrations, leave standstill after the regular hour centrifugal, precipitate with deionized water is redissolved, the rotary evaporation precipitation, and lyophilize obtains protein powder.
Chlorogenic acid is a kind of polar material, and is water-soluble, is soluble in ethanol, acetone, is slightly soluble in ethyl acetate.The proteinic aqueous solution, after adding ethanol, acetone and other organic solvent gradually, the remarkable reduction that the solubleness of protein in this system can be in various degree is precipitated out from solution.Use separable sunflower protein of water extraction and alcohol precipitation method and chlorogenic acid.
Beneficial effect of the present invention: equipment is simple, and operational safety is polluted few; Can improve oil yield efficiency, and the free oil quality that obtains is higher, is easy to refining; The enzymatic treatment mild condition can reclaim most protein from hydrolyzed solution; Oil is easily separated with residue, as adopting three-phase centrifuge separating oil, hydrolyzed solution and residue, can improve the device processes ability greatly; Effectively separated albumen and chlorogenic acid, separation method is simple, the protein powder quality height of gained, and color and luster is good.
Description of drawings
Fig. 1 aqueous enzymatic extraction sunflower seed oil and reclaim proteic process flow diagram.
Embodiment
Embodiment 1
The shelling sunflower seeds carries out dry ground with medicinal herb grinder.Sunflower seeds 150g after pulverizing is added the 0.05mol/L citrate buffer solution of 750mlpH4.8, stir evenly the complex cellulase that adds 2.5% (w/w shelling sunflower seeds butt meter) after the form slurry, at 50 ℃ of following enzymolysis 7h.Centrifugal with 3000rpm, obtain free oil, emulsus liquid layer, hydrolyzed solution and precipitation after centrifugal.The careful emulsus liquid layer that takes out carries out secondary centrifuging, and centrifugal force is 8000g, with separating of oil come out in the emulsus liquid layer.Calculate the free oil yield, can reach 87%.
Get the hydrolyzed solution after 200ml filters, vacuum concentration to solid content is about 13%, adds 600ml-20 ℃ dehydrated alcohol protein precipitation approximately, 3000rpm is centrifugal after leaving standstill certain hour, precipitate with deionized water is redissolved, and the rotary evaporation in vacuo precipitation obtains protein powder after the lyophilize.The chlorogenic acid rate of removing is 84%, and protein recovery reaches 80%, and protein powder is creamy white.
Embodiment 2
The shelling sunflower seeds carries out dry ground with medicinal herb grinder.Sunflower seeds 150g after pulverizing is added the 0.05mol/L citrate buffer of 750mlph4.8, stir evenly the complex cellulase that adds 2% (w/w shelling sunflower seeds butt meter) after the form slurry, at 50 ℃ of following enzymolysis 5h.Centrifugal with 3000rpm, obtain free oil, emulsus liquid layer, hydrolyzed solution and precipitation after centrifugal.The careful emulsus liquid layer that takes out carries out secondary centrifuging, and centrifugal force is 8000g, with separating of oil come out in the emulsus liquid layer.Calculate the free oil yield, can reach 80%.
Get the hydrolyzed solution after 200ml filters, vacuum concentration to solid content is about 9%, adds 200ml-20 ℃ dehydrated alcohol protein precipitation approximately, 3000rpm is centrifugal after leaving standstill certain hour, precipitate with deionized water is redissolved, and the rotary evaporation in vacuo precipitation obtains protein powder after the lyophilize.The chlorogenic acid rate of removing is 80%, and protein recovery reaches 60%, and it is faint yellow that protein powder is.
Embodiment 3
The shelling sunflower seeds carries out dry ground with medicinal herb grinder.Sunflower seeds 150g after pulverizing is added the 0.05mol/L citrate buffer of 900mlpH4.8, stir evenly the complex cellulase that adds 1% (w/w shelling sunflower seeds butt meter) after the form slurry, at 50 ℃ of following enzymolysis 5h.Centrifugal with 3000rpm, obtain free oil, emulsus liquid layer, hydrolyzed solution and precipitation after centrifugal.The careful emulsus liquid layer that takes out carries out secondary centrifuging, and centrifugal force is 8000g, with separating of oil come out in the emulsus liquid layer.Calculate the free oil yield, can reach 78%.
Get the hydrolyzed solution after 200ml filters, vacuum concentration to solid content is about 15%, adds 370ml-20 ℃ dehydrated alcohol protein precipitation approximately, 3000rpm is centrifugal after leaving standstill certain hour, precipitate with deionized water is redissolved, and the rotary evaporation in vacuo precipitation obtains protein powder after the lyophilize.The chlorogenic acid rate of removing is 82%, and protein recovery reaches 69%, and it is faint yellow that protein powder is.
Claims (2)
1. an aqueous enzymatic extraction sunflower seed oil and reclaim method of protein, it is characterized in that with the shelling sunflower seeds be raw material, after dry ground, add citrate buffer, carry out enzyme digestion reaction with complex cellulase, it is centrifugal that enzymolysis finishes the back, obtain free oil, milk sap, hydrolyzed solution and grouts, the milk sap that obtains is through high speed centrifugation, the part of reentrying free oil, hydrolyzed solution is after filtration, vacuum concentration, alcohol precipitation, centrifugal, precipitation and lyophilize reclaim and obtain protein, and technology is:
A) dry ground: pulverize the shelling sunflower seeds with medicinal herb grinder, destroy its histocyte;
B) enzymolysis process: the shelling sunflower seeds after the pulverizing in liquid/seed than w/w 3: 1-7: 1 ratio adds the 0.05mol/L citrate buffer of pH4.8, stir evenly the complex cellulase that adds after the form slurry in shelling sunflower seeds quality 1%-3%, temperature in the enzymolysis process is 50 ℃, stirring velocity is 250r/min, enzymolysis 5-7h, enzymolysis solution is directly centrifugal, centrifugal speed 3000r/min, separate and obtain free oil I, milk sap I, hydrolyzed solution and grouts, the milk sap I that obtains is carried out again centrifugal, centrifugal force is 8000g, separates to obtain free oil II and milk sap II, merge free oil I and free oil II, total free oil yield reaches 85%-90%;
C) reclaim protein: hydrolyzed solution after filtration, vacuum concentration is to the solid content of 9%-15%, is the 50%-75% ethanol sedimentation with-20 ℃ final concentrations, leaves standstill after the regular hour centrifugal, precipitate with deionized water is redissolved, and rotary evaporation takes off the ethanol postlyophilization and obtains protein powder.
2. method according to claim 1 is characterized in that used complex cellulase is the Viscozyme L of NOVO company.
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Cited By (18)
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| CN101974364A (en) * | 2009-09-27 | 2011-02-16 | 东北农业大学 | Method for extracting soybean grease from soybean emulsion |
| CN101455240B (en) * | 2008-12-29 | 2011-04-06 | 东北农业大学 | Pumpkin seed oil extraction method using water enzyme method |
| CN101235398B (en) * | 2008-03-05 | 2011-06-15 | 中国林业科学研究院亚热带林业研究所 | Technique for extracting residual oil from oil-tea camellia pomace by enzyme method |
| CN102199486A (en) * | 2011-03-23 | 2011-09-28 | 武汉普赛特膜技术循环利用有限公司 | Method for integrated utilizing sunflower seeds |
| CN102491898A (en) * | 2011-11-16 | 2012-06-13 | 中国农业科学院农产品加工研究所 | Method for simultaneously extracting chlorogenic acid and sunflower protein from sunflower seed meals |
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| CN105087134A (en) * | 2015-07-30 | 2015-11-25 | 江苏俊启粮油股份有限公司 | Sunflower seed oil aqueous enzymatic extraction method |
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| CN107125430A (en) * | 2017-03-10 | 2017-09-05 | 河南工业大学 | It is a kind of while the method for preparing oil body and non-hydrolyzed protein matter |
| CN109181844A (en) * | 2018-09-14 | 2019-01-11 | 许昌鑫瑞德化工科技有限公司 | A kind of modified vegetable and animals oils extracting method |
| CN112574811A (en) * | 2020-12-15 | 2021-03-30 | 佳格食品(厦门)有限公司 | Moderate processing method of sunflower seed oil |
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- 2006-10-18 CN CN 200610096926 patent/CN1952094A/en active Pending
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| CN101235398B (en) * | 2008-03-05 | 2011-06-15 | 中国林业科学研究院亚热带林业研究所 | Technique for extracting residual oil from oil-tea camellia pomace by enzyme method |
| CN101455240B (en) * | 2008-12-29 | 2011-04-06 | 东北农业大学 | Pumpkin seed oil extraction method using water enzyme method |
| CN101974364A (en) * | 2009-09-27 | 2011-02-16 | 东北农业大学 | Method for extracting soybean grease from soybean emulsion |
| CN101974364B (en) * | 2009-09-27 | 2012-10-31 | 东北农业大学 | Method for extracting soybean grease from soybean emulsion |
| CN102199486A (en) * | 2011-03-23 | 2011-09-28 | 武汉普赛特膜技术循环利用有限公司 | Method for integrated utilizing sunflower seeds |
| CN102491898B (en) * | 2011-11-16 | 2014-04-09 | 中国农业科学院农产品加工研究所 | Method for simultaneously extracting chlorogenic acid and sunflower protein from sunflower seed meals |
| CN102491898A (en) * | 2011-11-16 | 2012-06-13 | 中国农业科学院农产品加工研究所 | Method for simultaneously extracting chlorogenic acid and sunflower protein from sunflower seed meals |
| CN102703206A (en) * | 2012-06-19 | 2012-10-03 | 东北农业大学 | Method for extracting fragrant sunflower seed oil |
| CN102766526A (en) * | 2012-08-21 | 2012-11-07 | 东北农业大学 | Production method for synchronously extracting soybean oil and soybean powdered oil |
| CN103343046A (en) * | 2013-07-19 | 2013-10-09 | 东北农业大学 | Method for preparing oil and protein by cold pressing and enzymolysis of sesame |
| CN103436350A (en) * | 2013-07-20 | 2013-12-11 | 烟台大学 | Aqueous enzymatic method for extracting rapeseed oil and recovering protein |
| CN104531338A (en) * | 2015-01-05 | 2015-04-22 | 湖南紫苏科研有限公司 | Method for comprehensively extracting and refining perilla oil |
| CN105087134A (en) * | 2015-07-30 | 2015-11-25 | 江苏俊启粮油股份有限公司 | Sunflower seed oil aqueous enzymatic extraction method |
| CN105112154A (en) * | 2015-09-28 | 2015-12-02 | 江苏俊启粮油股份有限公司 | Aqueous enzymatic processing technology for peanut oil |
| CN105331438A (en) * | 2015-11-25 | 2016-02-17 | 江南大学 | Method for preparing rapeseed oil by using semi-solid aqueous enzymatic method |
| CN105331438B (en) * | 2015-11-25 | 2019-03-15 | 江南大学 | A kind of method that semisolid aqueous enzymatic method prepares rapeseed oil |
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| CN106398853A (en) * | 2016-09-12 | 2017-02-15 | 上海应用技术大学 | Extraction method of Chongming golden melon seed oil |
| CN107125430A (en) * | 2017-03-10 | 2017-09-05 | 河南工业大学 | It is a kind of while the method for preparing oil body and non-hydrolyzed protein matter |
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| CN112574811A (en) * | 2020-12-15 | 2021-03-30 | 佳格食品(厦门)有限公司 | Moderate processing method of sunflower seed oil |
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