CN101602979A - A kind of extracting method of soybean oil - Google Patents
A kind of extracting method of soybean oil Download PDFInfo
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Abstract
The invention discloses a kind of extracting method of soybean oil.May further comprise the steps: (1) soybean is pulverized back twin-screw extruder extruding puffing; (2) soy products behind the extruding puffing is mixed with water; Add proteolytic enzyme and carry out enzymolysis; (3) enzyme that goes out, centrifugation, promptly.The inventive method utilization is pulverized expelling-expansion pretreatment and is separated soybean oil with the method that biological enzyme combines, the oil in water emulsion that separation obtains need not refining and can obtain high-quality oil behind breakdown of emulsion, be of high nutritive value, but soybean protein and soybean peptides utility value height and less investment, the total oily extraction yield of the inventive method can reach 93.18%.The required equipment of the inventive method is simple, operational safety, gained soybean oil no solvent residue; in addition; the inventive method action condition gentleness; degraded product in the system does not react with extract; can protect the quality of each composition effectively; the inventive method can be from full fat soybean separating oil and protein simultaneously, the protein denaturation rate is low.
Description
Technical field
The present invention relates to a kind of extracting method of Vegetable oil lipoprotein, relate in particular to the extracting method of soybean oil, belong to the extraction manufacture field of Vegetable oil lipoprotein.
Background technology
Aqueous enzymatic method is to adopt biological enzyme hydrolyzed soy raw material, puies forward deep-fried twisted dough sticks spare gentleness, and the performance of oilseed protein changes hardly, no matter is the direct processing and utilization of aqueous phase, still reclaims protein isolate and utilizes, and effect is all very good.But water is the method for solvent extraction vegetables oil is applied to the oil plant to the such low oil content of soybean, and effect is relatively poor, and the grease extraction yield is low.And contained albumen is not only measured manyly in the soybean, and good quality is the elaboration in the vegetable-protein, therefore, solves the greasy difficult problem of low oil content soybean oil plant aqueous enzymatic extraction, and is significant.
Just there is the scholar that biotechnology (enzyme) is applied to grease to seek the more extracting method of science, health, safety abroad in the fifties in last century.To the nineties in last century, aqueous enzymatic method is proposed the concern that oil tech causes Chinese scholars once more, because the aqueous enzymatic method technology not only can overcome conventional oil-producing technique in many-sided drawbacks such as economy, environment, safety, and can effectively reclaim other nutritive substances in the oil plant in extract oil.The research of aqueous enzymatic extraction progressively becomes the focus of current domestic and international foodstuffs industry, nearly 20 kinds of oil plants is tested so far, and the enzyme that research relates to has nearly ten kinds.Experiment shows, all can improve oil yield to the aqueous enzymatic method oil-producing technique of multiple oil plant, improves the quality and the by product quality of oil.The aqueous enzymatic extraction technology is to utilize oil plant to obtain grease and the Perfected process of albumen simultaneously, but also be the bigger processing method of research difficulty, particularly for the oil plant (most typical is soybean) of low oil content, exist oil yield lower, and albumen and the formed milk sap of grease technical barrier such as be difficult to that breakdown of emulsion separates behind the enzymolysis.
1973-1977 Italy scientist Montedoro, G and Petruccioli, the research that G is correlated with to the Enzymatic Extraction sweet oil.1979, during Olsen applied to microbial protease Alcalase soybean oil and proteinic water law is separated, to discharge the oil of its all absorption, the yield that makes oil was near 60% with the enzyme liberating protein molecule, and proteinic yield is near 40%.When nineteen eighty-three U.S. Fullbook produces the solubility protolysate of trophicity with enzyme from the watermelon seed, find the carrying out along with hydrolysis, part oil is released.He has obtained expected effect with enzyme extract oil and protein from vegetable seed and soybean subsequently.McGlone in 1986, o.C. and Canales, A.L.M utilize the extraction Oleum Cocois of new enzyme process technology success.Malaysian scientist Cheah in 1987, S.C., Augustin, M.A. utilize the enzyme process success extraction plam oil.Thailand scientist Olsen in 1988, H.S. have studied the pre-test of various plants seed aqueous enzymatic method system oil.Dominguez in 1993 etc. carry out correlative study to utilizing aqueous enzymatic method to extract grease from soybean and sunflower seed, and normal hexane lixiviate soybean oil carried out correlative study after nineteen ninety-five, they handled enzyme again.Italian scientist Ranalli in 1994, A, and Costantini, N. utilize biotechnology to extract sweet oil, nineteen ninety-five Ranalli, A, and Costantini, N utilizes existing at that time technology and achievement in research further to study and introduces the influence of proteolytic ferment to the sweet oil extraction yield, they had analyzed proteolytic ferment and produce the physics of sweet oil and chemical property and proposed the influence of processing parameter to the sweet oil quality and quantity in 1996, and at the addition of proteolytic enzyme the influence of sweet oil yield were analyzed.Brazilian scientist Pereira-Freitas, Hartman in 1997 and Couri etc. are applied to wet method extruding and puffing technology behind the strip plate in the middle of the aqueous enzymatic extraction soybean oil first, they point out through the thermoplastic extrusion process, help enzyme pair cell structural damage effect, reduce nonhydratable phosphatide and promote protein denaturation, reduce stability of emulsion, thereby raising oil extracting rate, and studies show that through them the significant parameter that influences oil yield is: the sleeve temperature of extrusion machine and nib aperture, the material-water ratio in the enzymolysis process, enzyme concentration and enzymolysis time.The best squeezing parameter parameter that they draw is: the sleeve temperature is that 90 ℃, nib aperture are 6mm, enzymolysis time is that 6h, material-water ratio are that the addition of 1: 10 and enzyme is 6%w/w, utilizes above processing parameter that the aqueous enzymatic method oil extracting rate is brought up to about 88%.Sarker in 1998, B.C and Singh, B.P.N etc. carry out correlative study to the optimization of the enzymolysis process condition of aqueous enzymatic extraction rapeseed oil, and obtain corresponding parameters optimization.Picuric-Jovanovic in 1997 and K, Vrvaski etc. be to utilizing the extraction plum nucleolus oil of aqueous enzymatic method success, and 1 year they study the influence of a greasy processing condition of aqueous enzymatic extraction again to plum kernel oil oxidation stability.Calendar year 2001 Y.B.Che Man and Suhardiyono etc. with the extraction by the aqueous enzymatic method success of Alcalase proteolytic enzyme Rice pollard oil, he points out that the addition of enzyme has the greatest impact to Rice pollard oil and proteic extraction yield through the response surface analysis method, and hydrolysis temperature and enzymolysis time are not remarkable to its influence, and the method by the response surface optimizing and confirmatory experiment obtained maximum oil extracting rate be 79% and protein extracting ratio be 68%.
Comprehensive foreign study report can see that aqueous enzymatic method system oil only was confined to high oil-containing crop in the past in 2005, and less for low butyraceous soybean research.Sight being put into aqueous enzymatic method 2005-2008 U.S. scientist produces in the soybean oil, U.S. scientist B.P.Lamsala, P.A.Murphyb in 2006 and L.A.Johnsona, b with strip plate after wet method extruding preconditioning technique should have in the middle of the aqueous enzymatic extraction soybean oil, they utilize the soybean oil in the full fat soybean that extracts wet method extruding behind the strip plate behind the mixture enzymolysis of cellulase, proteolytic enzyme and two kinds of enzymes.It is 68% that the full fat soybean that pushes behind the evidence strip plate directly extracts its oil extracting rate of grease with aqua method, utilizes the aqueous enzymatic extraction soybean oil can make oil extracting rate bring up to 88% behind the adding proteolytic enzyme, and add cellulase oil extracting rate is had no significant effect.They analyze is that extruding can strengthen proteinic hydrolysis result free oil is discharged behind enzymolysis greatly behind the strip plate.B.P.Lamsal in 2007 and L.A.Johnson study the breakdown of emulsion of aqueous enzymatic extraction soybean oil, they point out that Recent study shows by after the expelling-expansion pretreatment behind the strip plate, the oil extracting rate that can make aqueous enzymatic method carry oil (prozyme) brings up to 88%, obtain three-phase after utilizing grease enzymolysis in the middle of the aqueous enzymatic extraction full fat soybean powder centrifugal: 1. 2. 3. hydrolyzed solution of milk sap of free oil, they draw and no matter use after the strip plate extruding pre-treatment aqueous enzymatic method or aqua method extracts soybean oil through research, the subunit of soybean protein all is present in and plays emulsifying effect in the milk sap, makes soybean oil be difficult to separate.They have carried out comparative study at above problem to hot breakdown of emulsion, freeze-thaw breakdown of emulsion and phosphatide enzyme process breakdown of emulsion, studies show that freeze-thaw demulsification the best, but complex process.The Phospholipid hydrolase demulsification technology is simple and effect is better, utilizes this method can make the recovery rate of free oil reach 70-80%.They have broken former aqueous enzymatic method and only have been fit to the restriction that high oil-containing crop is carried oil, make aqueous enzymatic method produce soybean oil become feasible (oil extracting rate is about 88%).
The technical study that oil is carried to aqueous enzymatic method by China is later relatively abroad.First enzyme process is produced soybean oil and soy bean protein hydrolysate simultaneously from full fat soybean technology was carried out preliminary study from Wuxi Light Industry Univ. in 1992.Route comprised for three steps: the first, thus take water extraction protein in the soybean and grease to be separated the purpose that reaches preliminary extraction protein and oil with insoluble sludge; Second step was that the grease of taking enzyme process to combine with protein is separated; The 3rd step was to prepare high-quality grease by breakdown of emulsion from oil in water emulsion.Its concrete operational path is seen Fig. 1.
From this operational path as can be seen, raw material does not carry out pre-treatment, and in extracting the grease process through twice enzymolysis, because the restriction of biological enzyme technology at that time, so only adopted Sumizyme MP and neutral protease to be hydrolyzed, and complex process, the grease extraction yield only can reach about 65%.Do not see relevant paper publishing because restrictions such as preconditioning technique, biological enzyme technology and demulsification technology are immature are domestic after 1994.Professor He Guoqing of Zhejiang University instructed doctoral candidate Qian Junqing that water enzyme organic solvent extraction soybean oil has been carried out systematic study in 2000, selection and the best enzymolysis process condition and the extraction conditions of best enzyme have been obtained through research, reaching about 84% of soybean oil extraction yield, but because technology limitation at that time, they do not break away from the use of organic solvent fundamentally to solve the difficult point of aqueous enzymatic extraction soybean oil.
The patent of invention of publication number CN101401658A discloses the middle method for testing of a kind of aqueous enzymatic extracting of peanut oil and protolysate, this method adopts the middle method for testing of aqueous enzymatic extracting of peanut oil and protolysate, it is raw material with the peanut, carry out enzymolysis with single Sumizyme MP, introduce three-phase separator separating oil simultaneously, oil-water mixture and undissolved residue, and use disc centrifuge that the oil-water mixture that separation obtains is further separated, obtain milk sap and hydrolyzed solution, wherein milk sap obtains breakdown of emulsion oil behind the freeze-thaw breakdown of emulsion, obtains peanut protolysate powder after hydrolyzed solution is spray-dried.This method is to be applicable to that this high oil-containing crop of peanut extracts oil-producing technique, and it is easier therefore to carry oil, and technology is simpler comparatively speaking, and what the pre-treatment of raw material was adopted is to carry out alkali after pulverizing to carry, and what breakdown of emulsion adopted is the breakdown of emulsion that thaws.
The soybean oil reparation technology has two kinds at present, and a kind of is solvent extraction method and extruding puffing-lixiviation process, and another kind is the mechanical expression method.The solvent extraction method that oil yield is bigger, dregs of rice residual oil content is low by (＜1%, butt), solvent has that some are residual, the composition of hydrogen gasoline often, be controlled on certain safe aspect as far as possible, but hardly sometimes on vernacular arts problematic words can cause residual or residual the exceeding standard of turnover oil of hydrogen oil.
Extract solvent for No. six and use solvent as main the leaching, its main component is normal hexane and heptane, contains objectionable impuritiess such as a small amount of benzene, toluene in addition, and nerve system of human body, internal organs are had certain injury, make lipoid dysequilibrium in the neurocyte, cause various function of human body disorders.Solvent residual amount is too high in the edible oil, and long-term eating can cause people's psychoplegia even paralysis.Another kind of solvent normal hexane membrane lipid is had damaging action, and the acute suction of normal hexane can cause or the injury response of enhancing body active oxygen radical, causes lipid peroxidation injury.
Wet dregs of rice sex change in high temperature precipitation process is serious, and has with an organic solvent increased the loaded down with trivial details property of technology, and facility investment is big, and energy consumption is big, reduces the security of producing, and causes environmental pollution.Protein denaturation is serious.
Milling process is the oil that pushes out by physics, also has other deliquescent thing also can come out, the sense organ of influence oil; Through later stage high temperature long time treatment, oil, cake are of poor quality, the residual oil content height in the dregs of beans (5%～7%, butt); Protein denaturation is serious in the dregs of beans, can only be used as fertilizer, and nutrition circle at present finds that after deliberation the soybean active peptide has very high nutritive value and functionally active (class morphine sample activity, hormone and adjusting functions of hormones widely, the intravital enzyme of biology had adjusting and inhibit feature, improve mineral substance transportation and absorption, antibiotic and viral, improve immunizing power, anti-oxidant, remove free radical anti-ageing and hypertension and hyperlipidemia etc.), so this method causes the proteic waste of a large amount of quality plants.
The new national Specification of putting into effect, a secondary leach salad oil dissolvent residual standard per kilogram must not surpass 10 milligrams, and three level Four should not surpass 50 milligrams, and this illustrates and still contains dissolvent residual in the qualified oil product.
The famous nutritionist's Adler doctor Davis research of the U.S. is recently pointed out, can prevent that without vitamin-E contained in the purified vegetables oil oxidation of carotene, suprarenin, sexual hormoue and vitamin A, D, K from destroying.But, the soybean oil of solvent extraction and mechanical expression gained must be passed through multiple tracks refining procedures such as alkali refining, depickling could be as food oils, and refining process can make some nutritive ingredient loss, and wherein vitamin-E is very easily oxidized, in refining oil, vitamin-E is all gone, dissolvent residual directly causes detrimentally affect to HUMAN HEALTH simultaneously, and is oxidized behind the oil and fat refining, though be difficult for corrupt, but can only energize, there are not other nutritive values.At present, solvent lixiviate and squeezing are made oil back dregs of beans mainly as feed, use seldom aspect food, and are only limited to fermentation food.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, and a kind of extracting method of new soybean oil is provided.
Technical problem to be solved by this invention is achieved through the following technical solutions:
A kind of extracting method of soybean oil may further comprise the steps: (1) soybean is pulverized the back and carries out extruding puffing with twin-screw extruder; (2) soy products behind the extruding puffing is mixed with water obtain mixed solution; In mixed solution, add proteolytic enzyme and carry out enzymolysis; (3) enzymolysis solution is gone out enzyme, centrifugation, promptly.
In order to reach better extraction effect, the institute soybean is adjusted into 10%-18% (w/w) (being preferably 14.5% (w/w)) extruding puffing again with its water ratio after pulverizing in the step (1); Wherein, described extruding puffing preferably carries out under the following conditions: the aperture of twin-screw extruder nib is preferably 14-26mm, more preferably 20mm; The twin-screw extruder screw speed is preferably 70-160r/min, more preferably 105r/min; Twin-screw extruder sleeve temperature is preferably 75 ℃-120 ℃, more preferably 90 ℃.
In the step (2), preferred, with the soy products behind the extruding puffing and water according to 1: the part by weight of 3.5-9 mixes, and is preferred, and its part by weight according to 1: 6.5 is mixed, and obtains mixed solution; The pH value of mixed solution is adjusted to 8-12, preferred, the pH value of mixed solution is adjusted to 9.5; The proteolytic enzyme that is added can be alkaline endo proteolytic enzyme, flavor protease, and papoid, compound protease or neutral protease are preferably Alcalase alkaline endo proteolytic enzyme; Wherein, by weight percentage, the consumption of the enzyme that is added is preferably the 1.2-3% that accounts for the reaction mixture gross weight, and more preferably 2%;
Wherein, described hydrolysis temperature is preferably 45 ℃-65 ℃, more preferably 57 ℃; Enzymolysis time is preferably 2-6 hour, more preferably 3 hours 45 minutes;
Centrifugal being preferably described in the step (3): centrifugal rotational speed is 4500r/min; Centrifugation time is 30min;
The inventive method is on the basis of Mechanical Crushing, adopt the enzyme of energy degrading plant oil plant cell or have the enzyme of Degradation to act on oil plant complex bodys such as lipoprotein, lipopolysaccharides, make grease be easy to from the oil plant solid, discharge, utilize non-oil component (albumen and carbohydrate) to the oil and the avidity difference of water, utilize profit proportion difference simultaneously and oil is separated with non-oil component.In the inventive method, enzyme is except complex bodys such as the oil plant cell of degrading, decomposition lipoprotein, lipopolysaccharides, can also destroy the lipoprotein membrane that is wrapped in oil droplets that oil plant forms in processes such as defibrination, reduce the stability of milk sap, thereby improve the free oil yield.
The inventive method utilization is pulverized expelling-expansion pretreatment and is separated soybean oil with the aqueous enzymatic method that biological enzyme combines, devices needed is simple, operational safety, gained soybean oil no solvent residue, the oil in water emulsion that separation obtains need not refining and can obtain high-quality oil behind breakdown of emulsion, be of high nutritive value, but soybean protein and soybean peptides utility value height and less investment.Through checking and simultaneous test, total oily extraction yield can reach about 93.18% under enzymolysis process condition of the present invention.
The inventive method action condition gentleness (normal temperature, organic solvent-free, no violent chemical reaction), the degraded product in the system generally can not react with extract, can protect grease, protein and colloid etc. can utilize the quality of composition effectively.
Aqueous enzymatic method of the present invention is produced soybean oil and is compared with traditional oil-producing technique and mainly have following technological advantage:
1. simultaneously separating oil and protein from full fat soybean.
2. simple, the operational safety of equipment, vegetables oil no solvent residue and less investment.
3. can remove beans raw meat composition, the nutrition inhibitor factor and the aerogenesis factor in the beans.
4. separate the soybean deep processed product of the solvable soy bean protein hydrolysate oil-containing of iso-electric point very high (about 90%) that obtains by enzyme process, can be widely used in the numerous food system.
5. the protein denaturation rate is low.
6. the oil in water emulsion that is obtained by the enzyme process separation need not to handle behind breakdown of emulsion and can obtain high-quality oil.
Description of drawings
The process route chart of the existing aqueous enzymatic extraction soybean oil of Fig. 1;
The process route chart of Fig. 2 the inventive method;
The kind of the different enzymes of Fig. 3 is to the influence of total oily extraction yield;
Fig. 4 enzyme concentration is to the influence of total oily extraction yield;
Fig. 5 hydrolysis temperature is to the influence of total oily extraction yield;
Fig. 6 enzymolysis time is to the influence of total oily extraction yield
Fig. 7 material-water ratio is to the influence of total oily extraction yield;
Fig. 8 pH is to the influence of total oily extraction yield;
Each factor of Fig. 9 is to investigating the Dimension Reduction Analysis figure of index;
Figure 10 Y=f (x
1, x
2) response surface;
Figure 11 Y=f (x
1, x
3) response surface;
Figure 12 Y=f (x
1, x
5) response surface;
Figure 13 Y=f (x
2, x
3) response surface;
Figure 14 Y=f (x
2, x
4) response surface;
Figure 15 Y=f (x
2, x
5) response surface;
Figure 16 Y=f (x
3, x
4) response surface;
Figure 17 Y=f (x
4, x
5) response surface;
The kind of the different enzymes of Figure 18 is to the influence of total oily extraction yield;
Each factor of Figure 19 is to investigating the Dimension Reduction Analysis figure of index;
Figure 20 Y=f (x
1, x
2) level line and response surface;
Figure 21 Y=f (x
1, x
3) level line and response surface;
Figure 22 Y=f (x
1, x
4) level line and response surface;
Figure 23 Y=f (x
2, x
3) level line and response surface;
Figure 24 Y=f (x
3, x
4) level line and response surface;
Embodiment
Further describe the present invention below in conjunction with specific embodiment, advantage of the present invention and characteristics will be more clear along with description.But these embodiment only are exemplary, scope of the present invention are not constituted any restriction.It will be understood by those skilled in the art that and down can make amendment or replace without departing from the spirit and scope of the present invention, but these modifications and replacing all fall within the scope of protection of the present invention the details of technical solution of the present invention and form.
The screening experiment of experimental example 1 hydrolysate of soybean protein processing condition optimum parameter
1 materials and methods
1.1 material, reagent
What soybean Heilungkiang Academy of Agricultural Sciences cultivated cultivates agricultural 42
Alcalase alkaline endo proteolytic enzyme Denmark novo company
Flavor protease Denmark novo company
Papoid Denmark novo company
Compound protease Denmark novo company
AS1398 neutral protease Denmark novo company
1.2 key instrument equipment
PHS-25 type acidometer Shanghai great achievement instrument plant
Electronic analytical balance Mei Lete-Tuo benefit instrument (Shanghai) Co., Ltd.
Whizzer Beijing Medical Centrifugal Machine Factory
Accurate electric blender Jiangsu Province Jintan City's high honour instrument Manufacturing Co., Ltd
Electric-heated thermostatic water bath Yuyao City east electric instrument factory
Semi-automatic azotometer Shanghai Xin Jia Electronics Co., Ltd.
Digestion instrument Shanghai Qianjian Instrument Co., Ltd.
Beater disintegrating machine China Tianjin Tai Site Instr Ltd.
Soxhlet extractor Tianjin Glass Instrument Factory
Twin-screw extruder MY146 * 2 Jiangsu shepherd groups
Screw diameter (mm) 146 main shaft power (kW) 315
Quality-adjusting device power (kw) 22 feeder power (kw) 2.2
1.3 experimental technique
1.3.1 the composition measurement of soybean
The mensuration of moisture: GB304-87 measures; The mensuration of crude fat: the Soxhlet extraction process is measured among the GB5512-85; The mensuration of crude protein: the GB6432-94 standard method is carried out; Determination of ash: GB5009.4-85; Material composition is measured: utilize near-infrared analyzer to measure
1.3.2 technical process
Soybean → cleaning → pulverizing → moisture adjusting → extruding puffing (nib aperture 18mm, 90 ℃ of sleeve temperature, material water ratio 14%, screw speed 100rpm) → pulverizing → adjusting pH value and the temperature → enzymolysis → enzyme that goes out → centrifugal → soybean oil
1.3.3 calculation formula
Total oily extraction yield (%)=(the used gram of raw soybeans count in the * soybean behind the massfraction-enzymolysis of oil in the residue resid amount)/used gram of raw soybeans is counted the massfraction of oil in the * soybean
2 results and discussion
2.1 the selection of enzyme
Take by weighing the full fat soybean 50g that pulverizes again through extruding puffing and place 5 four-necked bottles, by identical enzyme concentration, material-water ratio, enzymolysis time, with total oily extraction yield serves as to investigate index, fixing various proteolytic enzyme (Sumizyme MPs, neutral protease, papoid, compound protease, flavor protease) enzymolysis pH value and temperature (according to suggestion optimum pH and temperature on the trade mark), according to the fixing material-water ratio of the domestic and foreign literature of consulting, hydrolysis time all is fixed as 3h, and the addition at enzyme is 4000U/g respectively, 6000U/g, 8000U/g, 10000U/g, be hydrolyzed under the condition of 12000U/g.Select the kind of aqueous enzymatic extraction soybean oil enzyme after the most suitable expelling-expansion pretreatment, the results are shown in Figure 3.
By Fig. 3 result's Sumizyme MP advantage maximum as can be seen, so this experimental selection Sumizyme MP.
2.2 enzymolysis process list factor condition is to the influence of total oily extraction yield
2.2.1 the enzyme concentration of Sumizyme MP is to the influence of total oily extraction yield
Material-water ratio 1: 5, enzymolysis time 4h, 55 ℃ of hydrolysis temperatures, enzymolysis pH are 9, under the centrifugal 30min condition of 4500r/min, investigate the influence of enzyme concentration to total oily extraction yield, the results are shown in Figure 4.Obviously increase when enzyme concentration total oily extraction yield greater than 1.5% time as can be seen by Fig. 4 result, so the enzyme concentration level is selected 1.4-2.2% in the response surface test design below.
2.2.2 hydrolysis temperature is to the influence of total oily extraction yield
At enzyme concentration 2%, material-water ratio 1: 5, enzymolysis time 4h, enzymolysis pH are 9, under the centrifugal 30min condition of 4500r/min, investigate the influence of hydrolysis temperature to total oily extraction yield, the results are shown in Figure 5.By Fig. 5 result as can be seen near hydrolysis temperature total oily extraction yield 55 ℃ have higher value to occur because consider interaction, so hydrolysis temperature is chosen in 45-65 ℃ in the response surface test design below.
2.2.3 enzymolysis time is to the influence of total oily extraction yield
At enzyme concentration 2%, material-water ratio 1: 5,55 ℃ of hydrolysis temperatures, enzymolysis pH are 9, under the centrifugal 30min condition of 4500r/min, investigate the influence of enzymolysis time to total oily extraction yield, the results are shown in Figure 6.By Fig. 6 result as can be seen enzymolysis time obviously increase greater than the total oily extraction yield of 2h, but when enzymolysis time greater than 4h, total oily extraction yield does not have considerable change, so enzymolysis time is selected 2-4h in the response surface test design below.
2.2.4 material-water ratio is to the influence of total oily extraction yield
At enzyme concentration 2%, 55 ℃ of hydrolysis temperatures, enzymolysis time 4h, enzymolysis pH are 9, under the centrifugal 30min condition of 4500r/min, investigate the influence of material-water ratio to total oily extraction yield, the results are shown in Figure 7.By Fig. 7 result as can be seen material-water ratio obviously increase greater than 1: 4 total oily extraction yield, but when material-water ratio greater than 1: 8, total oily extraction yield is on a declining curve, so material-water ratio selects 1 in the response surface test design below: 4-1: 8.
2.2.5pH influence to total oily extraction yield
At enzyme concentration 2%, 55 ℃ of hydrolysis temperatures, enzymolysis time 4h, material-water ratio 1: 5 under the centrifugal 30min condition of 4500r/min, is investigated the influence of pH to total oily extraction yield, the results are shown in Figure 8.By Fig. 8 result as can be seen pH near 9-10, have higher value to occur, so pH selects 8.5-10.5 in the response surface test design below.
2.3 the response surface optimum experimental reaction conditions of enzymolysis process
2.3.1 empirical factor level code table
On the basis of single factor research, choosing enzyme concentration, hydrolysis temperature, enzymolysis time, material-water ratio and 5 factors of enzymolysis pH is independent variable(s), is response value with total oily extraction yield, according to the center combination principle of design, the experiment of design response surface analysis, its level of factor coding schedule sees Table 1.
Table 1 level of factor coding schedule
2.3.2 response surface experimental establishment and experimental result
This experimental applications response surface optimized method carries out process optimization.With x
1, x
2, x
3, x
4, x
5Being independent variable(s), is response value Y with total oily extraction yield, response surface experimental program and the results are shown in Table 2.Experiment 1-26 is factorial experiment, and 27-36 is 10 center tests, in order to the estimating experiment error.
Table 2 response surface experimental program and experimental result
2.3.3 response surface interpretation
Carry out data analysis by statistical analysis software SAS9.1, it is as follows to set up quadratic response face regression model:
Y=89.785+1.36x
1+ 0.658x
2+ 1.878x
3+ 1.265x
4+ 0.05x
5-0.486x
1 2-1.378x
1x
2-1.813x
1x
3-1.215x
1x
5-1.555x
2x
3+ 1.84x
2x
4+ 1.793x
2x
5-0.994x
3 2+ 0.93x
3x
4-1.691x
4 2+ 1.563x
4x
5-1.823x
5 2Regression analysis and The results of analysis of variance see Table 3, and the response surface optimizing sees Table 4, and Dimension Reduction Analysis is seen Fig. 8, and significant mutually alternately response surface analysis is seen Fig. 9-Figure 16.
Table 3 returns and The results of analysis of variance
Annotate: by analysis, the relative coefficient (R of total regression
2) be 96.24%, the coefficient of determination (R
2Adj) be 92.69%
As shown in Table 3, the linear relationship between equation dependent variable and the independent variable(s) is obvious, and this model returns significantly (p＜0.0001), and it is not remarkable to lose the plan item, and this model R
2=96.24%, R
2 Adj=92.69%, illustrate that this model and experimental fit are good, linear relationship is remarkable between independent variable(s) and the response value, and the theory that can be used for this reaction is inferred.Can obtain the factor contributions rate by the F check is: x
3＞x
1＞x
4＞x
2＞x
5, i.e. enzymolysis time＞enzyme concentration＞solid-liquid ratio＞hydrolysis temperature＞pH.Each factor is to investigating the rule that influences of the total oily extraction yield of index as seen from Figure 9.
Application responds face optimizing analytical procedure is analyzed regression model, seeks optimal response and the results are shown in Table 4, and working as enzyme concentration as shown in Table 4 is 2.04%, temperature is 57 ℃, and enzymolysis time is 2.87h, and material-water ratio is 1: 6.46, pH is 9.5, and response surface has optimum value 90.99524 ± 0.571%.
Table 4 response surface optimizing result
2.4 confirmatory experiment and simultaneous test
Under the top condition that the response surface analysis method is tried to achieve, promptly enzyme concentration is 2%, and temperature is 57 ℃, and enzymolysis time is 3h, and material-water ratio is 1: 6.5, and pH 9.5 carries out 3 parallel laboratory tests, and the mean value of 3 parallel laboratory tests of total oily extraction yield is 91.67%.Total oily extraction yield predictor is 90.99524 ± 0.571%.Experimental value and regression equation predictor that response value is described are coincide good.Utilizing the total oily extraction yield of traditional wet heat treatment method under identical enzymatic hydrolysis condition only is 72.54%.
3 experiment conclusion
The enzymolysis process parameter of the aqueous enzymatic extraction soybean oil after utilizing the response surface analysis method to expelling-expansion pretreatment is optimized.Having set up corresponding mathematical model is that later pilot scale and suitability for industrialized production provided fundamental basis, and to have obtained optimum enzymolysis process condition be that enzyme concentration is 2%, and temperature is 57 ℃, and enzymolysis time is 3h, and material-water ratio is 1: 6.5, and pH is 9.5.Through checking and simultaneous test as can be known under optimum enzymolysis process condition total oily extraction yield can reach about 91.67%, improved 19 percentage points than the total oily extraction yield of enzymolysis after traditional damp and hot pre-treatment.
The optimal process parameter of the pulverizing expelling-expansion pretreatment technology of raw material experiment before experimental example 2 enzymolysis
Based on experimental example 1 determined best aqueous enzymatic extraction soybean oil and proteic technology, carry out single factor squeeze test, determine the scope of each extruding puffing system parameter (sleeve temperature, nib aperture, screw speed, material water ratio).With total reducing sugar yield in oil extracting rate, protein extracting ratio, the hydrolyzed solution serves as to investigate index, carries out response surface and designs 5 hydraulic tests of 5 factors
2.2 key instrument equipment
PHS-25 type acidometer Shanghai great achievement instrument plant
Electronic analytical balance Mei Lete-Tuo benefit instrument (Shanghai) Co., Ltd.
Whizzer Beijing Medical Centrifugal Machine Factory
Accurate electric blender Jiangsu Province Jintan City's high honour instrument Manufacturing Co., Ltd
Electric-heated thermostatic water bath Yuyao City east electric instrument factory
Semi-automatic azotometer Shanghai Qianjian Instrument Co., Ltd.
Digestion instrument Shanghai Qianjian Instrument Co., Ltd.
Scanning electronic microscope company
Beater disintegrating machine China Tianjin Tai Site Instr Ltd.
Soxhlet extractor Tianjin Glass Instrument Factory
Twin-screw extruder MY146 * 2 Jiangsu shepherd groups
Screw diameter (mm) 146 main shaft power (kW) 315
Quality-adjusting device power (kw) 22 feeder power (kw) 2.2
2.3 experimental technique
1.3.1 the composition measurement of soybean
The mensuration of moisture: GB304-87 measures; The mensuration of crude fat: the Soxhlet extraction process is measured among the GB5512-85; The mensuration of crude protein: the GB6432-94 standard method is carried out; Determination of ash; GB5009.4-85; Material composition is measured: utilize near-infrared analyzer to measure
1.3.2 technical process
Soybean → cleaning → pulverizing → moisture adjusting → extruding puffing → pulverizing → adjusting pH value and temperature → enzymolysis (Alcalase alkaline endo proteolytic enzyme, processing condition are: enzyme concentration is 2%, temperature is 57 ℃, enzymolysis time is 3h40min, material-water ratio is 1: 6.5, and pH is 9.5) → enzyme → centrifugation of going out → soybean oil
↓ (residue is collected and is measured the Residual oil quality)
Soyabean polypeptide powder ← spraying drying ← soybean hydrolyzed solution, milk sap → breakdown of emulsion → soybean oil
1.3.3 calculation formula
1.3.4 the selection of extruding puffing system parameter
On the former study basis, the stability of comprehensive single factor experiment and twin-screw extruder, 12 central point responses of selected four factors, five levels curved design scheme sees Table 5
Table 5 level of factor coding schedule
2 results and discussion
2.1 raw material basal component
Table 6 raw soybeans main component
2.2 the selection of enzyme
Take by weighing the full fat soybean 50g that pulverizes again through extruding puffing respectively and place 5 four-necked bottles, by carrying out enzymolysis near identical enzyme concentration, material-water ratio, enzymolysis time and the suggestion enzymatic hydrolysis condition, with total oily extraction yield serves as to investigate index, select the kind of aqueous enzymatic extraction soybean oil enzyme after the most suitable expelling-expansion pretreatment, the results are shown in Figure 18.By Figure 18 result's Sumizyme MP advantage maximum as can be seen, so Sumizyme MP is selected in this research, with total oily extraction yield serves as that examination index protease hydrolysis condition is a factor, obtaining the optimum protein enzyme hydrolysis process is: enzyme concentration is 2%, temperature is 57 ℃, enzymolysis time is 3h, and material-water ratio is 1: 6.5, and pH is 9.5.Below test all adopts this technology to carry out enzymolysis.
2.3 response surface experimental establishment and experimental result
This experimental applications response surface optimized method carries out process optimization.With x
1, x
2, x
3, x
4Being independent variable(s), is response value Y with total oily extraction yield, response surface experimental program and the results are shown in Table 3.Experiment 1-24 is factorial experiment, and 25-36 is 12 center tests, in order to the estimating experiment error.
Table 7 response surface experimental program and experimental result
The response surface interpretation
Carry out data analysis by statistical analysis software SAS9.1, it is as follows to set up quadratic response face regression model:
(1) level value regression equation:
x
1, x
2, x
3, x
4Be the level of factor value
(2) actual value regression equation:
x
1, x
2, x
3, x
4Be the factor actual value
Regression analysis and The results of analysis of variance see Table 8, and Dimension Reduction Analysis is seen Figure 19, and Figure 20-Figure 24 is seen in significant mutually alternately response surface and level line analysis.
Table 8 returns and The results of analysis of variance
Annotate: by analysis, the relative coefficient (R of total regression
2) be 94.21%, the coefficient of determination (R
2Adj) be 90.34%, CV is 1.088296
As shown in Table 8, the linear relationship between equation dependent variable and the independent variable(s) is obvious, and this model recurrence is (p＜0.0001) significantly, and lose and intend item not remarkable (p＞0.05), and this model R
2=94.21%, R
2 Adj=90.34%, illustrate that this model and experimental fit are good, linear relationship is remarkable between independent variable(s) and the response value, and the theory that can be used for this reaction is inferred.Can obtain the factor contributions rate by the F check is: x
4＞x
1＞x
3＞x
2, i.e. sleeve temperature＞nib aperture＞screw speed＞material water ratio.
Each factor is to investigating the rule that influences of the total oily extraction yield of index as seen from Figure 19.Total oily extraction yield is with nib aperture x
1Increase increase earlier and afterwards change not quite.The total protein extraction yield is with material water ratio x
2Increase increase afterwards earlier and reduce.The total protein extraction yield is with screw speed x
3Increase, changing little back earlier increases.The total protein extraction yield increases earlier with the sleeve temperature and increases, after sharply reduce.
Application responds face optimizing analytical procedure is analyzed regression model, and working as the nib aperture as can be known is 20mm, and material water ratio is 14.5%, and screw speed is 105r/min, and the sleeve temperature is 90 ℃, and response surface has optimum value 93.02 ± 0.29%.
2.4 confirmatory experiment and simultaneous test
Under the top condition that the response surface analysis method is tried to achieve, promptly enzyme concentration 2%, 57 ℃ of temperature, and enzymolysis time 3h45min, material-water ratio 1: 6.5, pH9.5 carry out 3 parallel laboratory tests, and the mean value of 3 parallel laboratory tests of total oily extraction yield is 93.18%.Experimental value and regression equation predictor that response value is described are coincide good.Utilizing the total oily extraction yield of traditional wet heat treatment method under identical enzymatic hydrolysis condition only is 72.54%.
Claims (10)
1, a kind of extracting method of soybean oil may further comprise the steps: (1) soybean is pulverized the back and carries out extruding puffing with twin-screw extruder; (2) soy products behind the extruding puffing is mixed with water obtain mixed solution; In mixed solution, add proteolytic enzyme and carry out enzymolysis; (3) enzymolysis solution is gone out enzyme, centrifugation obtains the free soybean oil.
2, according to the described extracting method of claim 1, it is characterized in that: by weight percentage, in the step (1) soybean being pulverized back adjustment water ratio is 10%-18%, is preferably 14.5%.
3, according to the described extracting method of claim 1, it is characterized in that: described extruding puffing carries out under following processing parameter: the aperture of twin-screw extruder nib is 14-26mm; The twin-screw extruder screw speed is 70-160r/min; Twin-screw extruder sleeve temperature is 75 ℃-120 ℃.
4, according to the described extracting method of claim 3, it is characterized in that: described extruding puffing carries out under following processing parameter: the aperture of twin-screw extruder nib is 20mm; The twin-screw extruder screw speed is 105r/min; Twin-screw extruder sleeve temperature is 90 ℃.
5, according to the described extracting method of claim 1, it is characterized in that: in the step (2) with the soy products behind the extruding puffing and water according to 1: the part by weight of 3.5-9 mixes, and obtains mixed solution; Preferably, the soy products behind the extruding puffing is mixed with the part by weight of water according to 1: 6.5, obtain mixed solution.
6, according to the described extracting method of claim 1, it is characterized in that: the pH value with mixed solution in the step (2) is adjusted to 8-12, and is preferred, and the pH value of mixed solution is adjusted to 9.5.
7, according to the described extracting method of claim 1, it is characterized in that: the proteolytic enzyme that is added in the step (2) is selected from alkaline endo proteolytic enzyme, flavor protease, papoid, compound protease or neutral protease; Be preferably Alcalase alkaline endo proteolytic enzyme.
8, according to the described extracting method of claim 7, it is characterized in that: by weight percentage, the consumption of the enzyme that is added accounts for the 1.2-3% of reaction mixture gross weight, is preferably 2%.
9, according to the described extracting method of claim 1, it is characterized in that: the hydrolysis temperature described in the step (2) is 45 ℃-65 ℃, is preferably 57 ℃; Enzymolysis time is 2-6 hour, is preferably 3 hours 45 minutes.
10, according to the described extracting method of claim 1, it is characterized in that: the centrifugal rotational speed described in the step (3) is 4500r/min; Centrifugation time is 30min.
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