CN102703206A - Method for extracting fragrant sunflower seed oil - Google Patents
Method for extracting fragrant sunflower seed oil Download PDFInfo
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- CN102703206A CN102703206A CN2012102166623A CN201210216662A CN102703206A CN 102703206 A CN102703206 A CN 102703206A CN 2012102166623 A CN2012102166623 A CN 2012102166623A CN 201210216662 A CN201210216662 A CN 201210216662A CN 102703206 A CN102703206 A CN 102703206A
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Abstract
The invention discloses a method for extracting a fragrant sunflower seed oil and belongs to the extraction processing technique of plant fat. The method comprises the following steps: (1) frying cleaned sunflower seeds; (2) carrying out extrusion puffing pre-treatment to the fried sunflower seeds to obtain pressed fragrant sunflower oil and a puffed product; (3) mixing the puffed product obtained in the step (2) with water to obtain mixed solution, adding compound cellulose to the mixed solution to enzymatically hydrolyze and obtain an enzymatic hydrolysate; (4) enzyme-inactivating the enzymatic hydrolysate and centrifugally separating to obtain the free fragrant sunflower seed oil. According to the method of extracting the fragrant sunflower seed oil, the sunflower seed oil is separated in a method of combining frying, extrusion puffing pretreatment and bio-enzyme; after the emulsified oil subjected to separation is demulsified, the oil of high quality can be obtained without refining and has high nutritional value; the total oil extraction rate is up to 96.98 percent; the action conditions are mild and degradation products in the system are not reacted with the extract, so that the qualities of various components can be protected effectively.
Description
Technical field
The invention belongs to the extraction processing technology of Vegetable oil lipoprotein, relate in particular to a kind of process for extracting of giving off a strong fragrance sunflower seed oil.
Background technology
At present, the oily mechanize oil plant complete processing that is adopted of sunflower seeds system is progressively to grow up from the oil plants processing of five sixties heavy handicraft workshop and semi-mechanization production.Sunflower seeds oil-producing technique process is: shelling, press for extracting juice in advance, leaching.Sunflower seeds lixiviation process oil-producing technique and equipment are processed identical with soybean, vegetable seed.
Milling process also is physics system oil process, and it produces vegetables oil through technologies such as former abrasive lapping, squeezing, refinings.Lixiviation process is also claimed chemistry system oil process, and it produces vegetables oil through technologies such as raw material crushing, solvent soaking, precipitation, refinings.Press a lixiviation process in advance with two step combinations, improve oil yield.
Milling process can keep the flavour of product, but this method residual oil content is high, 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.
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 increase the loaded down with trivial details property of technology, the security that has reduced production and eaten, and caused environmental pollution; Micro-organic solvent residual in the processed oil has harm to human health.
The grouts of gained are generally used for extracting sunflower protein behind the sunflower seeds system oil, and the sunflower seed degreased dreg is that good feed is used protein resource.But sunflower seeds receives the effect of heating, machinery and solvent in the oily process of system, make the variation of protein generation physics, chemistry and biological aspect, has influenced protein quality.
Aqueous enzymatic method technology is on the basis of Mechanical Crushing; Adopt can degrading plant oil plant cell walls enzyme, or complex bodys such as lipoprotein, LPS are had the enzyme of Degradation, comprise cellulase, polygalacturonase, glycase, proteolytic enzyme etc.; Act on oilseed; Make grease be easy to from oilseed, discharge, utilize non-oil component (protein and glucide), utilize profit proportion difference simultaneously and oil is separated with non-oil component the oil and the avidity difference of water.In the aqueous enzymatic method technology; Enzyme is except complex bodys such as the oilseed cell of degrading, decomposition lipoprotein, LPS; Can also destroy the lipoprotein membrane that is wrapped in oil droplets that oilseed forms in processes such as defibrination, reduce the stability of milk sap, thereby improve the free oil yield.
Along with the development of oil prodution industry in modern age, people explore a kind of new oil extracting methods aqua method one by one.In the fifties in last century, aqua method is proposed the alternative oil extracting process as the solvent extraction method owing to safer and economical.Compare with traditional squeezing, lixiviation process, aqua method has unique advantage: can oil be separated with protein simultaneously, gentle processing conditions can make protein keep higher nutritive value and functional property.But mechanical shear stress that oilseed is applied owing to aqua method and calendering force are not enough to thoroughly destroy cell walls and cause that oil yield is low, protein recovery is not high; Oil yield is lower when being used for the lower oilseed of oleaginousness (like soybean); Part oil and protein bound make very easily oxidative rancidity of product.
In vegetable oil material, grease is present in the vegetable oil material cell, and combines with other macromole (protein and glucide) usually to exist, and constitutes complex bodys such as lipoprotein, LPS.Have only cellularstructure and grease compounded body to destroy, could extract grease wherein oil plant.Therefore, explore the cellularstructure how thoroughly to destroy oil plant and grease compounded body improving oil yield, and effectively reclaim the key point that nutritive substance such as protein has become oil preparation process simultaneously.In mid-term in last century, people observe, and through the oil plant that enzyme is handled, oil yield is significantly improved, but economic factors has stoped its industrial applications.To the seventies, along with application and the popularization of microbial technique in enzyme is produced, the big volume production enzyme of industriallization has reduced the zymin price, uses the enzyme extraction Vegetable oil lipoprotein and has caused external many scholars' interest again.Nineteen eighty-three Fullbook has obtained desired result with enzyme stripping oil and protein from Semen Brassicae campestris and soybean.After the nineties, the research that enzyme process separates component such as grease and protein in the oil plant becomes the focus of domestic and international concern day by day, and in oil plants such as coconut, rice bran, vegetable seed, olive peanut, is applied.For rapeseed oil, Oleum Cocois, sweet oil, the experiment on laboratory, pilot scale and plant size all had report.China is later to this Study on Technology report, from Wang Zhang in 1994, professor Xu Shiying at home reported first since the aqueous enzymatic extraction VT 18, this The Application of Technology only limits to oil plants such as soybean, maize germ, vegetable seed and peanut.People such as J.Sineiro had carried out the greasy experiment of aqueous enzymatic extraction with different enzyme reaction time, water seed ratio and enzyme seed comparison sunflower seeds in 1997, had obtained optimal condition, though oil extracting rate is not high, its result helps to screen more effective enzyme.
Summary of the invention
Technical problem to be solved by this invention is exactly the deficiency to above-mentioned prior art, and a kind of process for extracting of giving off a strong fragrance sunflower seed oil is provided, and reaches the raising oil yield, and makes the high giving off a strong fragrance sunflower seed oil purpose of nutritive value composition.
Technical problem to be solved by this invention realizes through following technical scheme,
A kind of process for extracting of giving off a strong fragrance sunflower seed oil, this method may further comprise the steps: (1) will be passed through the sunflower seeds of cleaning and propagandize processing hotly, and propagandizing temperature hotly is 20-120 ℃, and the time of propagandizing hotly is 10-50min, goes out pot temperature 120-140 ℃; (2) sunflower seeds after will propagandizing hotly carries out expelling-expansion pretreatment; Obtain squeezing giving off a strong fragrance sunflower seed oil and expanded product, described sunflower seeds water ratio is 7%-11%, and the aperture of nib is 10-18mm; Screw speed is 30-50r/min, and the sleeve temperature is 80 ℃-120 ℃; (3) the expanded product that step (2) is obtained mixes with water and obtains mixed solution; Said expanded product and water weight ratio are 1: 3-9; In mixed solution, add complex cellulase and carry out enzymolysis and obtain enzymolysis solution, enzymolysis time is 1-7h, and enzymolysis pH is 3-7; Hydrolysis temperature is 40-60 ℃, and enzyme concentration is the 1.5-3.5% of weight of material; (4) with the enzymolysis solution enzyme that goes out, spinning obtains free giving off a strong fragrance sunflower seed oil, and described centrifugal rotational speed is 4500r/min, and centrifugation time is 30min.
Preferred sunflower seeds is propagandized parameter hotly and is: propagandizing temperature hotly is 105 ℃, and the time of propagandizing hotly is 34min, and going out pot temperature is 133 ℃.
Preferred expanded parameter is: the sunflower seeds water ratio is 9.25%, and the aperture of nib is 15mm, and screw speed is 41r/min, and the sleeve temperature is 100 ℃.
Preferred parameter is: expanded product and water weight ratio are 1: 6.5.
Preferred enzymolysis parameter is: hydrolysis temperature is 47 ℃, and enzymolysis time is 5.2h, and enzyme concentration is 2.4% of a weight of material, and enzymolysis pH is 4.9.
The inventive method is on the basis of Mechanical Crushing; Adopt the enzyme of ability degrading plant oil plant cell or have the enzyme of Degradation to act on oil plant complex bodys such as lipoprotein, LPS; Make grease be easy to from the oil plant solid, discharge; Utilize non-oil component (albumen and glucide) 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, LPS; 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.
Aqueous enzymatic method of the present invention is produced sunflower seed oil and is compared with traditional oil-producing technique and mainly have following technological advantage:
1. simple, the operational safety of equipment, vegetables oil no solvent residue and less investment.
2. separate the sunflower seeds deep processed product of the solvable sunflower seeds X 1000 of the iso-electric point oil-containing very high (about 90%) that obtains by enzyme process, can be widely used in the numerous food system.
3. the protein denaturation rate is low.
Description of drawings
The process route chart of Fig. 1 the inventive method;
Fig. 2 propagandizes the influence of temperature to total oily extraction yield hotly;
Fig. 3 propagandizes the influence of time to total oily extraction yield hotly;
Fig. 4 goes out the influence of pot temperature to total oily extraction yield;
Fig. 5 propagandizes factor hotly to investigating the Dimension Reduction Analysis figure of index;
Fig. 6 propagandizes temperature hotly and propagandizes mutual response surface of time hotly;
Fig. 7 propagandizes temperature hotly and goes out the mutual response surface of pot temperature;
Fig. 8 propagandizes the time hotly and goes out the mutual response surface of pot temperature;
The kind of the different enzymes of Fig. 9 is to the influence of total oily extraction yield;
Figure 10 enzyme concentration is to the influence of total oily extraction yield;
Figure 11 hydrolysis temperature is to the influence of total oily extraction yield;
Figure 12 enzymolysis time is to the influence of total oily extraction yield;
Figure 13 solid-liquid ratio is to the influence of total oily extraction yield;
Figure 14 pH is to the influence of total oily extraction yield;
Figure 15 enzymolysis factor is to investigating the Dimension Reduction Analysis figure of index;
Figure 16 Y=f (X
1, X
3) response surface;
Figure 17 Y=f (X
2, X
3) response surface;
Figure 18 Y=f (X
4, X
5) response surface;
Figure 19 Y=f (X
2, X
5) response surface;
Figure 20 Y=f (X
2, X
4) response surface;
Figure 21 Y=f (X
1, X
2) response surface;
Figure 22 extruding puffing factor is to investigating the Dimension Reduction Analysis figure of index;
Figure 23 Y=f (X
1, X
2) response surface;
Figure 24 Y=f (X
1, X
4) response surface;
Figure 25 Y=f (X
2, X
4) response surface;
Figure 26 Y=f (X
3, X
4) response surface;
Embodiment
Further describe the present invention below in conjunction with specific embodiment.
A kind of process for extracting of giving off a strong fragrance sunflower seed oil, this method may further comprise the steps: (1) will be passed through the sunflower seeds of cleaning and propagandize processing hotly, and propagandizing temperature hotly is 20-120 ℃, and the time of propagandizing hotly is 10-50min; (2) sunflower seeds after will propagandizing hotly carries out expelling-expansion pretreatment; Obtain squeezing giving off a strong fragrance sunflower seed oil and expanded product, described sunflower seeds water ratio is 7%-11%, and the aperture of nib is 10-18mm; Screw speed is 30-50r/min, and the sleeve temperature is 80 ℃-120 ℃; (3) the expanded product that step (2) is obtained mixes with water and obtains mixed solution; Said expanded product and water weight ratio are 1: 3-9; In mixed solution, add complex cellulase and carry out enzymolysis and obtain enzymolysis solution, enzymolysis time is 1-7h, and enzymolysis pH is 3-7; Hydrolysis temperature is 40-60 ℃, and enzyme concentration is the 1.5-3.5% of weight of material; (4) with the enzymolysis solution enzyme that goes out, spinning obtains free giving off a strong fragrance sunflower seed oil, and described centrifugal rotational speed is 4500r/min, and centrifugation time is 30min.
Preferred sunflower seeds is propagandized parameter hotly and is: propagandizing temperature hotly is 105 ℃, and the time of propagandizing hotly is 34min.
Preferred expanded parameter is: the sunflower seeds water ratio is 9.25%, and the aperture of nib is 15mm, and screw speed is 41r/min, and the sleeve temperature is 100 ℃.
Preferred parameter is: expanded product and water weight ratio are 1: 6.5.
Preferred enzymolysis parameter is: hydrolysis temperature is 47 ℃, and enzymolysis time is 5.2h, and enzyme concentration is 2.4% of a weight of material, and enzymolysis pH is 4.9.
Experimental example 1 is propagandized the screening experiment of processing condition optimum parameter hotly
1 materials and methods
1.1 material, reagent
1.3 experimental technique
1.3.1 technical process
Sunflower seeds → clear up → propagandize hotly → moisture adjusting → extruding puffing (nib aperture 15mm, 100 ℃ of sleeve temperature, material water ratio 9.25%, screw speed 41r/min) → pulverizing → adjusting pH value and the temperature → enzymolysis → enzyme that goes out → centrifugal → sunflower seed oil
1.3.2 calculation formula
Total oily extraction yield (%)=(the used gram of raw material sunflower seeds count in the * sunflower seeds behind the massfraction-enzymolysis of oil in the residue resid amount)/used gram of raw material sunflower seeds is counted the massfraction of oil in the * sunflower seeds
2 results and discussion
2.1 propagandize of the influence of the single factor condition of technology hotly to total oily extraction yield
2.1.1 propagandize the influence of temperature hotly to total oily extraction yield
Sunflower seeds after the cleaning is put into and propagandized pot hotly, and propagandizing temperature hotly is the investigation factor, is propagandizing time 30min hotly, goes out to propagandize sunflower seeds when pot temperature is 130 ℃ hotly, investigates and propagandizes the influence of temperature to total oily extraction yield hotly, and the result sees Fig. 2.Can find out that by Fig. 2 result total oily extraction yield obviously increases when propagandizing temperature greater than 80 ℃ hotly, select 80-120 ℃ so response surface test design mid-early stage is below propagandized temperature levels hotly.
2.1.2 propagandize the influence of time hotly to total oily extraction yield
Sunflower seeds after the cleaning is put into and propagandized pot hotly, is 100 ℃ propagandizing temperature hotly, and going out pot temperature is 130 ℃, investigates the influence of propagandizing total oily extraction yield of time hotly, and the result sees Fig. 3.Can find out that by Fig. 3 result near the time of propagandizing hotly total oily extraction yield 30min has higher value to occur, because consider interaction, so propagandize selection of time hotly at 20-40min in the response surface test design below.
2.1.3 go out the influence of pot temperature to total oily extraction yield
Sunflower seeds after the cleaning is put into and propagandized pot hotly; Propagandizing temperature hotly is 100 ℃; The time of propagandizing hotly is 30min; Investigate out the influence of pot temperature to total oily extraction yield, the result sees Fig. 4. can find out that by Fig. 4 result total oily extraction yield obviously increases when pot temperature greater than 120 ℃, be chosen in 120-140 ℃ so go out pot temperature 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 and propagandize temperature hotly, propagandizing the time hotly, go out 3 factors of pot temperature is independent variable(s), is response value with total oily extraction yield, according to the center combination principle of design, and the experiment of design response surface analysis,
Its level of factor coding schedule is seen table 1.
Table 1 level of factor coding schedule
2.3.2 response surface EE and experimental result
This experimental applications response surface optimized method carries out process optimization.With x
1, x
2, x
3Being independent variable(s), is response value Y with total oily extraction yield, and response surface experimental program and result see table 2.Experiment 1-14 is factorial experiment, and 15-20 is 6 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 through statistical analysis software SAS9.1, it is following to set up quadratic response face regression model: Y=91.58799+3.639347x
1+ 7.930939x
2+ 0.419009x
3-3.129769x
1 2-1.5975x
1x
2+ 1.67x
1x
3-4.625304x
2 2+ 1.1725x
2x
3-1.651913x
3 2
Regression analysis and The results of analysis of variance are seen table 3, and table 4 is seen in the response surface optimizing, and Dimension Reduction Analysis is seen Fig. 5, and significant mutually alternately response surface analysis is seen Fig. 6-8.
Table 3 recurrence and The results of analysis of variance
Annotate: through analyzing the relative coefficient (R of total regression
2) be 99.09%, the coefficient of determination (R
2Adj) be 98.27%
Can be known that by table 3 linear relationship between equation dependent variable and the independent variable(s) is obvious, this regression models is (p＜0.0001) significantly, and it is not remarkable to lose the plan item, and this model R
2=99.09%, R
2 Adj=98.27%, explain 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
2＞x
1＞x
3, time of promptly propagandizing hotly＞propagandize hotly temperature＞go out pot temperature.
Application responds face optimizing analytical procedure is analyzed regression model, seeks the optimal response result and sees table 4, can know that by table 4 propagandizing temperature hotly is 105 ℃, and the time of propagandizing hotly is 34min, and going out pot temperature is 133 ℃, and response surface has optimum value 96.12013 ± 0.612189%.
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 propagandizing temperature hotly is 105 ℃, and the time of propagandizing hotly is 34min, and going out pot temperature is 133 ℃, carries out 3 parallel laboratory tests, and the MV of 3 parallel laboratory tests of total oily extraction yield is 95.98%.Total oily extraction yield predictor is 96.12013 ± 0.612189%.Experimental value and regression equation predictor that response value is described are identical good.
3 experiment conclusion
Utilize the response surface analysis method to optimize to propagandizing processing parameter hotly the early stage of the enzymolysis process material of aqueous enzymatic extraction Trisun Oil R 80.Having set up corresponding mathematical model is that later pilot scale and suitability for industrialized production provided fundamental basis, and has obtained optimum and propagandize processing condition hotly for early stage, to propagandize temperature hotly be 105 ℃, and the time of propagandizing hotly is 34min, and going out pot temperature is 133 ℃.Can know that through checking and simultaneous test total oily extraction yield can reach about 95.98 under optimum enzymolysis process condition.
The screening experiment of experimental example 2 sunflower seeds enzymolysis process condition optimum parameters
1 materials and methods
1.1 material, reagent
1.3 experimental technique
1.3.1 the composition measurement of sunflower seeds
Moisture determination: GB5497-85 measures; Protein determination: GB5511-85 measures; Fat test: GB5512-85 measures; Total sugar determination: phenolsulfuric acid method; Determination of ash: GB5505-85 measures; Robust fibre is measured: GB/T6434-94 measures.
1.3.2 technical process
Sunflower seeds → cleaning → pulverizing → moisture adjusting → extruding puffing (nib aperture 15mm, 100 ℃ of sleeve temperature, material water ratio 9.25%, screw speed 41r/min) → pulverizing → adjusting pH value and the temperature → enzymolysis → enzyme that goes out → centrifugal → sunflower seed oil
1.3.3 calculation formula
Total oily extraction yield (%)=(the used gram of raw material sunflower seeds count in the * sunflower seeds behind the massfraction-enzymolysis of oil in the residue resid amount)/used gram of raw material sunflower seeds is counted the massfraction of oil in the * sunflower seeds
2 results and discussion
2.1 the selection of enzyme
Take by weighing the sunflower seeds 50g that pulverizes again through extruding puffing and place 5 four-necked bottles; By identical enzyme concentration, solid-liquid ratio, enzymolysis time; With total oily extraction yield serves as to investigate index; The enzymolysis pH value of fixing various proteolytic enzyme (cellulase, neutral protease, papoid, complex cellulase, Sumizyme MP) and temperature (according to advising optimum pH and temperature on the trade mark), according to the fixing solid-liquid ratio of the domestic and foreign literature of consulting, hydrolysis time and being hydrolyzed under the condition of right enzyme concentration.Select the kind of aqueous enzymatic extraction sunflower seed oil enzyme after the most suitable expelling-expansion pretreatment, the result sees Fig. 9.Can find out complex cellulase and proteolytic enzyme advantage maximum by Fig. 9 result, so this experimental selection complex cellulase.
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
Solid-liquid ratio 1: 5, enzymolysis time 4.5h, 50 ℃ of hydrolysis temperatures, enzymolysis pH are 4.8, under the centrifugal 30min condition of 4500r/min, investigate the influence of enzyme concentration to total oily extraction yield, the result sees Figure 10.Can be found out when enzyme concentration total oily extraction yield greater than 2% time by Figure 10 result obviously increases, so the enzyme concentration level is selected 2-2.8% in the response surface test design below.
2.2.2 hydrolysis temperature is to the influence of total oily extraction yield
At enzyme concentration 2.5%, solid-liquid ratio 1: 5, enzymolysis time 4.5h, enzymolysis pH are 4.8, under the centrifugal 30min condition of 4500r/min, investigate the influence of hydrolysis temperature to total oily extraction yield, the result sees Figure 11.Can find out that by Figure 11 result near hydrolysis temperature total oily extraction yield 50 ℃ has higher value to occur, because consider interaction, so hydrolysis temperature is chosen in 40-60 ℃ in the response surface test design below.
2.2.3 enzymolysis time is to the influence of total oily extraction yield
At enzyme concentration 2.5%, solid-liquid ratio 1: 5,50 ℃ of hydrolysis temperatures, enzymolysis pH are 4.8, under the centrifugal 30min condition of 4500r/min, investigate the influence of enzymolysis time to total oily extraction yield, the result sees Figure 12.Can find out that by Figure 12 result enzymolysis time obviously increases greater than the total oily extraction yield of 3h, but work as enzymolysis time greater than 5h, total oily extraction yield does not have considerable change, so enzymolysis time is selected 3.5-5.5h in the response surface test design below.
2.2.4 solid-liquid ratio is to the influence of total oily extraction yield
At enzyme concentration 2.5%, 50 ℃ of hydrolysis temperatures, enzymolysis time 4.5h, enzymolysis pH are 4.8, under the centrifugal 30min condition of 4500r/min, investigate the influence of solid-liquid ratio to total oily extraction yield, the result sees Figure 13.Can find out that by Fig. 7 result solid-liquid ratio obviously increases greater than 1: 4 total oily extraction yield, but work as solid-liquid ratio greater than 1: 8, total oily extraction yield is on a declining curve, so solid-liquid 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 2.5%, 50 ℃ of hydrolysis temperatures, enzymolysis time 4.5h, solid-liquid ratio 1: 5 under the centrifugal 30min condition of 4500r/min, is investigated the influence of pH to total oily extraction yield, and the result sees Figure 14.Can find out that by Figure 14 result pH has higher value to occur near 4-5, so pH selects 3.5-5.5 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, solid-liquid ratio and an enzymolysis pH5 factor 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 is seen table 5.
Table 5 level of factor coding schedule
2.3.2 response surface EE 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, and response surface experimental program and result see table 6.Experiment 1-26 is factorial experiment, and 27-36 is 10 center tests, in order to the estimating experiment error.
Table 6 response surface experimental program and experimental result
2.3.3 response surface interpretation
Carry out data analysis through statistical analysis software SAS9.1, it is following to set up quadratic response face regression model: Y=94.785+1.97x
1+ 1.815x
3+ 1.519x
4+ 1.379x
5-2.524x
1x
2-1.923x
1x
3-1.649x
2x
3+ 1.952x
2x
4+ 1.107x
2x
5-0.923x
3 2-1.662x
4 2+ 1.924x
4x
5-1.139x
5 2Regression analysis and The results of analysis of variance are seen table 7, and table 8 is seen in the response surface optimizing, and Dimension Reduction Analysis is seen Figure 15, and significant mutually alternately response surface analysis is seen Figure 16-Figure 21.
Table 7 recurrence and The results of analysis of variance
Annotate: through analyzing the relative coefficient (R of total regression
2) be 96.12%, the coefficient of determination (R
2Adj) be 90.94%
Can be known that by table 3 linear relationship between equation dependent variable and the independent variable(s) is obvious, this regression models is (p＜0.0001) significantly, and it is not remarkable to lose the plan item, and this model R
2=96.12%, R
2 Adj=90.94%, explain 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
1＞x
3＞x
4＞x
5＞x
2, i.e. enzyme concentration＞enzymolysis time＞solid-liquid ratio＞pH＞hydrolysis temperature.
Application responds face optimizing analytical procedure is analyzed regression model, seeks the optimal response result and sees table 8, can know that by table 8 working as enzyme concentration is 2.4%; Temperature is 47 ℃, and enzymolysis time is 5.26h, and solid-liquid ratio is 1: 6.56; PH is 4.9, and response surface has optimum value 97.45972 ± 1.044%.
Table 8 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 2.4%, and temperature is 47 ℃, and enzymolysis time is 5.26h, and solid-liquid ratio is 1: 6.56, and pH is 4.9, carries out 3 parallel laboratory tests, and the MV of 3 parallel laboratory tests of total oily extraction yield is 96.98%.Total oily extraction yield predictor is 97.45972 ± 1.044%.Experimental value and regression equation predictor that response value is described are identical good.
3 experiment conclusion
The enzymolysis process parameter of the aqueous enzymatic extraction Trisun Oil R 80 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 2.4%, and temperature is 47 ℃, and enzymolysis time is 5.26h, and solid-liquid ratio is 1: 6.56, and pH is 4.9.Can know that through checking and simultaneous test total oily extraction yield can reach about 96.98 under optimum enzymolysis process condition.
The optimal process parameter of the pulverizing expelling-expansion pretreatment technology of raw material experiment before experimental example 3 enzymolysis
Based on experimental example 2 determined best aqueous enzymatic extraction sunflower seed oil and proteic technologies, carry out single factor squeeze test, confirm the scope of each extruding puffing system parameter (sleeve temperature, nib aperture, screw speed, material water ratio).With total oily extraction yield serves as to investigate index, carries out response surface and designs 5 hydraulic tests of 4 factors
1 materials and methods
1.1 material, reagent
2.2
1.3 experimental technique
1.3.1 technical process
Sunflower seeds → clear up → propagandize hotly → moisture adjusting → extruding puffing → pulverizing → adjusting pH value and temperature → enzymolysis (complex cellulase; Processing condition are: enzyme concentration is 2.4%; Temperature is 47 ℃; Enzymolysis time is 5.2h, and solid-liquid ratio is 1: 6.5, and pH is 4.9) → enzyme → spinning of going out → sunflower seed oil
1.3.2 calculation formula
Total oily extraction yield (%)=(the used gram of raw material sunflower seeds count in the * sunflower seeds behind the massfraction-enzymolysis of oil in the residue resid amount)/used gram of raw material sunflower seeds is counted the massfraction of oil in the * sunflower seeds
1.3.3 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 is seen table 9
Table 9 level of factor coding schedule
2 results and discussion
2.1 response surface EE 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, and response surface experimental program and result see table 10.Experiment 1-24 is factorial experiment, and 25-36 is 12 center tests, in order to the estimating experiment error.
Table 10 response surface experimental program and experimental result
2.2 response surface interpretation
Carry out data analysis through statistical analysis software SAS9.1, it is following to set up quadratic response face regression model: Y=90.280+0.73x
1-0.875x
4-0.519x
1 2+ 0.631x
1x
2-1.758x
1x
3+ 1.282x
1x
4-1.173x
2 2+ 2.113x
2x
3+ 0.719x
3x
4-1.393x
4 2Regression analysis and The results of analysis of variance are seen table 11, and Dimension Reduction Analysis is seen Figure 22, and Figure 23-Figure 26 is seen in significant mutually alternately response surface and level line analysis.
Table 11 recurrence and The results of analysis of variance
Annotate: through analyzing the relative coefficient (R of total regression
2) be 94.21%, the coefficient of determination (R
2Adj) be 90.36%.
Can be known that by table 11 linear relationship between equation dependent variable and the independent variable(s) is obvious, this regression models 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=90.36%, explain 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.Application responds face optimizing analytical procedure is analyzed regression model, can know that material water ratio is 9.25% as nib aperture 15mm, and screw speed is 41r/min, and the sleeve temperature is 100 ℃, and response surface has optimum value 90.30 ± 0.29%.
2.3 confirmatory experiment and simultaneous test
Under the top condition that the response surface analysis method is tried to achieve, promptly solid-liquid ratio is 1: 6.5, and hydrolysis temperature is 47 ℃; Enzymolysis time is 5.2h; Enzyme concentration is 2.4%, and enzymolysis pH carries out 3 parallel laboratory tests under 4.9 conditions, and the MV of 3 parallel laboratory tests of total oily extraction yield is 91.18%.Experimental value and regression equation predictor that response value is described are identical good.
Claims (5)
1. the process for extracting of a giving off a strong fragrance sunflower seed oil, it is characterized in that this method may further comprise the steps: (1) will be passed through the sunflower seeds of cleaning and propagandize processing hotly, and propagandizing temperature hotly is 20-120 ℃, and the time of propagandizing hotly is 10-50min, goes out pot temperature 120-140 ℃; (2) sunflower seeds after will propagandizing hotly carries out expelling-expansion pretreatment; Obtain squeezing giving off a strong fragrance sunflower seed oil and expanded product, described sunflower seeds water ratio is 7%-11%, and the aperture of nib is 10-18mm; Screw speed is 30-50r/min, and the sleeve temperature is 80 ℃-120 ℃; (3) the expanded product that step (2) is obtained mixes with water and obtains mixed solution; Said expanded product and water weight ratio are 1: 3-9; In mixed solution, add complex cellulase and carry out enzymolysis and obtain enzymolysis solution, enzymolysis time is 1-7h, and enzymolysis pH is 3-7; Hydrolysis temperature is 40-60 ℃, and enzyme concentration is the 1.5-3.5% of weight of material; (4) with the enzymolysis solution enzyme that goes out, spinning obtains free giving off a strong fragrance sunflower seed oil, and described centrifugal rotational speed is 4500r/min, and centrifugation time is 30min.
2. the process for extracting of a kind of giving off a strong fragrance sunflower seed oil according to claim 1, it is characterized in that preferred sunflower seeds propagandizes parameter hotly and be: propagandizing temperature hotly is 105 ℃, and the time of propagandizing hotly is 34min, and going out pot temperature is 133 ℃.
3. the process for extracting of a kind of giving off a strong fragrance sunflower seed oil according to claim 1, it is characterized in that preferred expanded parameter is: the sunflower seeds water ratio is 9.25%, and the aperture of nib is 15mm, and screw speed is 41r/min, and the sleeve temperature is 100 ℃.
4. the process for extracting of a kind of giving off a strong fragrance sunflower seed oil according to claim 1 is characterized in that preferred parameter is: expanded product and water weight ratio are 1: 6.5.
5. the process for extracting of a kind of giving off a strong fragrance sunflower seed oil according to claim 1, it is characterized in that preferred enzymolysis parameter is: hydrolysis temperature is 47 ℃, and enzymolysis time is 5.2h, and enzyme concentration is 2.4% of a weight of material, and enzymolysis pH is 4.9.
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