CN102229852A - Method for extracting fatty acid balanced soybean blend oil - Google Patents
Method for extracting fatty acid balanced soybean blend oil Download PDFInfo
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Abstract
The invention relates to a method for extracting fatty acid balanced soybean blend oil, belonging to the field of vegetable oil and fat processing. The method comprises the following steps of: (1) mixing soybeans, peanuts, flaxseeds and tea seeds in proportion; (2) smashing a mixed oil material, and extruding and puffing by virtue of a screw extruder; (3) mixing the mixed oil material and water after extruding and puffing, and carrying out enzymolysis with protease; and (4) inactivating enzyme, demulsifying, and carrying out centrifugal separation, thus the fatty acid balanced soybean blend oil is obtained. In the invention, the soybeans and other oils are firstly mixed in proportion, and a method combining smashing, extruding and puffing as well as biological enzyme is utilized to separate oil, the obtained emulsified oil is demulsified and is not required to be refined, and high-quality and fatty acid balanced blend oil can be obtained. In the invention, the total oil extraction efficiency can reach 91.18%, only one production line is required to directly prepare the fatty acid balanced blend oil, oil and proteins can be simultaneously separated from the mixed oil material, and protein denaturation rate is low.
Description
Technical field
The invention belongs to the extraction manufacture field of Vegetable oil lipoprotein, relate in particular to raw material and mix the greasy method of back extraction.
Background technology
Edible oil by sources is divided into animal oil and vegetables oil, and animal oil is based on saturated fatty acid, and excessive meeting causes atherosclerosis; Vegetables oil is substantially free of cholesterol based on unsaturated fatty acids, and the kind of vegetables oil is also a lot, and nutritive value has nothing in common with each other.The edible oil of people's current consumption mainly contains: sunflower seed oil, peanut oil, soybean oil, rapeseed oil, Deng oil product by single raw material processing, often eat single certain oil, thereby can cause the insufficiency of intake of certain or several lipid acid or excessive. the intravital metabolic balance of people is changed, cause various diseases.Scientific and reasonablely balancedly take in diverse lipid acid,, keep persistent health to be absolutely necessary keeping the good function of tissue.Chinese Soclety of Nutrition recommend and in the world relatively approval be saturated fatty acid: monounsaturated fatty acids: polyunsaturated fatty acid=1: 1: 1, wherein polyunsaturated fatty acid n-6: n-3=(4～6): 1.Present common s-generation mixed oil on the Chinese market, with saturated fatty acid: monounsaturated fatty acids: polyunsaturated fatty acid=0.27: 1: 1, the n-6 polyunsaturated fatty acid: n-3 polyunsaturated fatty acid=5: 1 is a feature.Cause is subjected to the influence of the lipid acid that other food provided except that edible oil, and the difference of various places food habits, and also be mean value at 0.27: 1: 1,
Traditional mixed oil method all is that compound lard allocates making its lipid acid reach balance again to compound lard then after earlier single grease being proposed, and this method quantities is big, and production line is too much during suitability for industrialized production, the production cost height.And all will all will carry out index determining to every kind of grease, workload is big at every turn.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, for satisfying the human diet nutritional needs, provides a kind of extracting method of soybean mixed oil of new fatty acid balance.
Technical problem to be solved by this invention is achieved through the following technical solutions:
1, a kind of soybean mixed oil extracting method of fatty acid balance may further comprise the steps:
(1) soybean and peanut, linseed oil, tea seed are mixed in proportion to such an extent that mix oil plant, the shared per-cent of each composition is by weight: the soybean addition is 49%, peanut addition 28.5%, linseed oil addition 14.4%, tea seed addition 8.1%;
(2) the mixing oil plant that obtains in the above-mentioned steps (1) being pulverized the back handles with the screw extruder extruding puffing, mixing oil plant water content after the pulverizing is adjusted into 18%-22%, the aperture of screw extruder nib is 16-24mm, the screw extruder screw speed is 70-130r/min, and screw extruder sleeve temperature is 65 ℃-95 ℃;
(3) the mixing oil plant after the extruding puffing processing in the step (2) is mixed with water, obtain mixed solution, mixed solution massfraction 15%-25%, the pH value of mixed solution is adjusted to 8-10, add proteolytic enzyme and carry out enzymolysis, by weight percentage, the proteolytic enzyme consumption that is added accounts for the 1.3-2.1% of reaction mixture gross weight, hydrolysis temperature is 45 ℃-65 ℃, and enzymolysis time is 2-6 hour;
(4) introduce go out enzyme and centrifugation and handle finishing mixed solution that enzymolysis obtains in the step (3), promptly get the soybean mixed oil product of fatty acid balance, centrifugal rotational speed is 4500r/min; Centrifugation time is 30min.
2, mixing the oil plant water ratio after preferred the pulverizing is 20%, and the aperture of screw extruder nib is 22mm, and the screw extruder screw speed is 110r/min, and screw extruder sleeve temperature is 81 ℃.
3, mix the mixed solution massfraction that obtains with water be 22.5% to the mixing oil plant behind the preferred extruding puffing, and the pH value of mixed solution is 8.1, and it is 1.88% that the proteolytic enzyme consumption accounts for the mixture total weight amount, and hydrolysis temperature is 48 ℃, and enzymolysis time is 3 hours 30 minutes.
The principle of design of the present invention is that the fatty acid ratio of edible oil is designed to meet Chinese Soclety of Nutrition to the absorption ratio of the meals total fatty acids of Chinese residents promptly: saturated fatty acid: monounsaturated fatty acids: polyunsaturated fatty acid=(0～1): 1: 1, and n-6 polyunsaturated fatty acid: n-3 polyunsaturated fatty acid=(4～6): 1.Three kinds of fatty acid ratios are as far as possible near 0.27: 1: 1.In order to solve the fatty acid ratio imbalance problem that single natural fats and oils exists, the present invention is a major ingredient with common soybean, with peanut, tea seed, linseed oil auxiliary material, after being mixed in proportion earlier, mix oil plant and carry out extruding puffing is produced fatty acid balance in conjunction with biological enzyme mixed oil
The inventive method original creation is mixed in proportion raw material earlier, produces mixed oil by extruding puffing combination water enzyme process then, makes it once to carry the mixed oil that the oil back just can be satisfied high quality and fatty acid balance simultaneously.This method gained mixed oil no solvent residue separates the oil in water emulsion obtain and need not refining can obtain high-quality oil behind breakdown of emulsion, is of high nutritive value, and fatty acid balance, and mix in the oil plant separating oil and protein simultaneously, the protein denaturation rate is low.Only need a production line can directly produce the mixed oil of fatty acid balance, save the energy, the protection environment is saved cost, can realize suitability for industrialized production
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.Through checking and simultaneous test, total oily extraction yield can reach about 91.18% 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.And only utilize a technical process just can finish greasy extraction.
The present invention compares with tradition system mixed oil technology mainly has following technological advantage:
1. proportioning raw materials is mixed, and only can finish the extraction grease with a production line, significantly reduces cost.
2. simple, the operational safety of equipment, vegetables oil no solvent residue and less investment.
3. simultaneously separating oil and protein.
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, directly reaches fatty acid balance, satisfies human diet balance.
Description of drawings
Fig. 1-1 overall process route
Mutual level line analysis of Fig. 1-2 mixture experiment design factor to the fatty acid distribution influence;
Fig. 2-1 enzyme concentration is to the influence of total oily extraction yield
Fig. 2-2 hydrolysis temperature is to the influence of total oily extraction yield
Fig. 2-3 enzymolysis time is to the influence of total oily extraction yield
Fig. 2-4 solid-liquid ratio is to the influence of total oily extraction yield
Fig. 2-5 enzymolysis ph is to the influence of total oily extraction yield
Each enzymolysis parameter of Fig. 2-6 is to the Dimension Reduction Analysis of fatty acid distribution
Mutual significantly the response surface analysis of each enzymolysis parameter of Fig. 2-7 to fatty acid distribution
Each enzymolysis parameter of Fig. 2-8 is to the Dimension Reduction Analysis of total oily extraction yield
Mutual significantly the response surface analysis of each enzymolysis parameter of Fig. 2-9 to total oily extraction yield
Each enzymolysis parameter of Fig. 2-10 is to fuzzy evaluation result's Dimension Reduction Analysis
Each extruding puffing parameter of Fig. 3-1 is to the Dimension Reduction Analysis of fatty acid distribution
Mutual significantly the response surface analysis of each extruding puffing parameter of Fig. 3-2 to fatty acid distribution
Each extruding puffing parameter of Fig. 3-3 is to the Dimension Reduction Analysis of total oily extraction yield
Mutual significantly the response surface branch of each extruding puffing parameter of Fig. 3-4 to total oily extraction yield
Each extruding puffing parameter of Fig. 3-5 is to fuzzy evaluation result's Dimension Reduction Analysis
Embodiment
Further describe the present invention below in conjunction with specific embodiment:
1, a kind of soybean mixed oil extracting method of fatty acid balance may further comprise the steps:
(1) soybean and peanut, linseed oil, tea seed are mixed in proportion to such an extent that mix oil plant, the shared per-cent of each composition is by weight: the soybean addition is 49%, peanut addition 28.5%, linseed oil addition 14.4%, tea seed addition 8.1%;
(2) the mixing oil plant that obtains in the above-mentioned steps (1) being pulverized the back handles with the screw extruder extruding puffing, mixing oil plant water content after the pulverizing is adjusted into 18%-22%, the aperture of screw extruder nib is 16-24mm, the screw extruder screw speed is 70-130r/min, and screw extruder sleeve temperature is 65 ℃-95 ℃;
(3) the mixing oil plant after the extruding puffing processing in the step (2) is mixed with water, obtain mixed solution, mixed solution massfraction 15%-25%, the pH value of mixed solution is adjusted to 8-10, add proteolytic enzyme and carry out enzymolysis, by weight percentage, the proteolytic enzyme consumption that is added accounts for the 1.3-2.1% of reaction mixture gross weight, hydrolysis temperature is 45 ℃-65 ℃, and enzymolysis time is 2-6 hour;
(4) introduce go out enzyme and centrifugation and handle finishing mixed solution that enzymolysis obtains in the step (3), promptly get the soybean mixed oil product of fatty acid balance, centrifugal rotational speed is 4500r/min; Centrifugation time is 30min.
2, mixing the oil plant water ratio after preferred the pulverizing is 20%, and the aperture of screw extruder nib is 22mm, and the screw extruder screw speed is 110r/min, and screw extruder sleeve temperature is 81 ℃.
3, mix the mixed solution massfraction that obtains with water be 22.5% to the mixing oil plant behind the preferred extruding puffing, and the pH value of mixed solution is 8.1, and it is 1.88% that the proteolytic enzyme consumption accounts for the mixture total weight amount, and hydrolysis temperature is 48 ℃, and enzymolysis time is 3 hours 30 minutes.
The mixing match experiment of experimental example 1 raw material
Method of the present invention is that soybean, peanut, linseed oil, tea seed are mixed earlier by a certain percentage, and the grease that the compound aqueous enzymatic method is produced just meets fatty acid balance.Do not need each oil plant to carry the oil back and be in harmonious proportion proportioning.Satisfy saturated fatty acid: monounsaturated fatty acids: polyunsaturated fatty acid=(0-1): 1: 1, near 0.27: 1: 1, n-6 polyunsaturated fatty acid: n-3 polyunsaturated fatty acid=4-6: 1.Guarantee monounsaturated fatty acids: polyunsaturated fatty acid=1: 1
1 materials and methods
1.1 material, reagent
Soybean, peanut, linseed oil, tea seed
Protamex 6L Sumizyme MP 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
GC-2010 type gas chromatograph (day island proper Tianjin company)
Multiple oil plant synchronized mixes machine self-control
Twin-screw extruder MY146 * 2
Screw diameter (mm) 146 main shaft power (kW) 315
Quality-adjusting device power (kw) 22 feeder power (kw) 2.2 Jiangsu shepherd groups
1.3 experimental technique
1.3.1 the composition measurement of every kind of oil plant
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 lipid acid is measured (GB/T17376-2008)
1.3.3 technical process
See accompanying drawing 1-1
1.3.4 data processing
Carry out mixture experiment design with design expert software
2 results and discussion
2.1 determining of enzymatic hydrolysis condition and various oil plant addition scopes
So the present invention is main foundation with the soybean mixed oil that other oil plant allotments make the mixing oil plant directly produce fatty acid balance as main raw material with soybean aqueous enzymatic method system oil, enzymolysis under protamex 6L Sumizyme MP optimum enzymolysis condition, the enzymolysis process parameter is: enzyme concentration 1.85%, 50 ℃ of hydrolysis temperatures, enzymolysis time 3.6h, material-water ratio 1: 6, enzymolysis pH value 9.26.Mixing the oil plant pretreatment process is in the method extruding puffing, and the extruding puffing parameter of the most suitable aqueous enzymatic extraction soybean oil is: nib aperture 20mm, material water ratio 14.5%, screw speed 105r/min, 90 ℃ of sleeve temperature.
2.2 the different additions of every kind of oil carry out process optimization to this experimental applications of batch mixing experimental study mixture experiment design method of fatty acid distribution scale effect.With total compound 500g is standard, the factor of representing respectively with A (soybean addition %), B (peanut addition %), C (linseed oil addition %), D (tea seed addition %) is an independent variable(s), with fatty acid ratio not is dependent variable, satisfy saturated fatty acid: monounsaturated fatty acids: polyunsaturated fatty acid=(0-1): 1: 1, near 0.27: 1: 1, n-6 polyunsaturated fatty acid: n-3 polyunsaturated fatty acid=4-6: 1.Guarantee monounsaturated fatty acids: polyunsaturated fatty acid=1: 1.Mixture experiment design experimental program and the results are shown in Table 1-1
Table 1-1 test arrangement and result
2.2.1 every kind of different additions of oil plant influence interpretation of result to fatty acid ratio
Carry out data analysis by statistical analysis software design expert, it is as follows to set up regression model:
R1＝0.62829A+1.45983B+0.39629C+6.63238D-1.03117AB-0.15455AC-10.17604AD-1.76142BC-3.99209BD-10.11547CD+1.57687ABC+22.90052ABD+43.94587ACD-6.36526BCD
Return with The results of analysis of variance and see Table 1-2, Fig. 1-2 is seen in interactive level line analysis, and the mixture experiment design optimum result sees Table 1-3.
Table 1-2 returns and The results of analysis of variance
By showing 1-2 as can be known, the linear relationship between equation dependent variable and the independent variable(s) is obvious, and this model returns significantly (p＜0.001), and it is not remarkable to lose the plan item, and this model R
2=99.22%, R
2 Adj=98.35%, 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: AD＞AC＞BC＞AC＞BC.
Table 1-3 mixture experiment design optimum result
As show 1-3 and have 25 groups of experimental programs can the bonding unsaturated fatty acids as can be seen: polyunsaturated fatty acid=1: 1.Through experimental verification, like this really, and experimental bias is not remarkable, illustrates that our regression equation fitness is good.
2.2.2 confirmatory experiment
From these 25 groups optimum experimental group, find, satisfy saturated fatty acid: monounsaturated fatty acids: polyunsaturated fatty acid=(0-1): 1: 1, near 0.27: 1: 1, n-6 polyunsaturated fatty acid: n-3 polyunsaturated fatty acid=4-6: 1.Through repeatedly experimental verification, the 15th group of experiment meets the demands, and saturated fatty acid: monounsaturated fatty acids: polyunsaturated fatty acid can reach 0.31: 1: 1, the n-6 polyunsaturated fatty acid: the n-3 polyunsaturated fatty acid was near 5: 1.Final definite soybean addition is 49%, peanut addition 28.5%, linseed oil addition 14.4%, tea seed addition 8.1%.
The screening experiment of experimental example 2 hydrolysate of soybean protein processing condition optimum parameters
1 materials and methods
1.1 material, reagent
Soybean, peanut, linseed oil, tea seed
Protamex 6L Sumizyme MP 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
GC-2010 type gas chromatograph (day island proper Tianjin company)
Multiple oil plant synchronized mixes machine self-control
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 technical process
Mix oil plant → 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 → mixed oil
1.3.2 lipid acid is measured (GB/T17376-2008)
2 results and discussion
2.1 enzymolysis process list factor condition is to the influence of fatty acid distribution
2.1.1 the enzyme concentration of Sumizyme MP is to the influence of fatty acid distribution
At material-water ratio 20%, 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 fatty acid distribution, the results are shown in Table 2-1.By table 2-1 result as can be seen when enzyme concentration single unsaturated fatty acids 1.7% time: polyunsaturated fatty acid approaches 1 most, so enzyme concentration level selection 1.3-2.1% in the response surface test design below.
Table 2-1 enzyme concentration is to the influence of fatty acid distribution
2.1.2 hydrolysis temperature is to the influence of fatty acid distribution
At enzyme concentration 2%, material-water ratio 20%, enzymolysis time 4h, enzymolysis pH is 9, under the centrifugal 30min condition of 4500r/min, investigate the influence of hydrolysis temperature to fatty acid distribution, the results are shown in Table near 2-2 result's hydrolysis temperature saturated fatty acid 55 ℃ as can be seen: monounsaturated fatty acids: polyunsaturated fatty acid=(0-1): 1: 1, approaching, n-6 polyunsaturated fatty acid: n-3 polyunsaturated fatty acid=4-6: 1, because consider interaction, so hydrolysis temperature is chosen in 45-65 ℃ in the response surface test design below.
Table 2-2 hydrolysis temperature is to the influence of fatty acid distribution
2.1.3 enzymolysis time is to the influence of fatty acid distribution
At enzyme concentration 2%, material-water ratio 20%, 55 ℃ of hydrolysis temperatures, enzymolysis pH are 9, under the centrifugal 30min condition of 4500r/min, investigate the influence of enzymolysis time to fatty acid distribution, the results are shown in Table 2-3.By table 2-3 result as can be seen enzymolysis time just can satisfy saturated fatty acid when the 3h: monounsaturated fatty acids: polyunsaturated fatty acid=(0-1): 1: 1, near 0.27: 1: 1, n-6 polyunsaturated fatty acid: n-3 polyunsaturated fatty acid=4-6: 1, changing greater than 3h is not clearly, so enzymolysis time is selected 2-4h in the response surface test design below.
Table 2-3 enzymolysis time is to the influence of fatty acid distribution
2.1.4 material-water ratio is to the influence of fatty acid distribution
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 fatty acid distribution, the results are shown in Table 2-4.By 2-4 result as can be seen material-water ratio satisfied saturated fatty acid at 25% o'clock: monounsaturated fatty acids: polyunsaturated fatty acid=(0-1): 1: 1, near 0.27: 1: 1, n-6 polyunsaturated fatty acid: n-3 polyunsaturated fatty acid=4-6: 1, so material-water ratio is selected 15%-35% in the response surface test design below
Table 2-4 solid-liquid ratio is to the influence of fatty acid distribution
2.1.5pH influence to fatty acid distribution
At enzyme concentration 2%, 55 ℃ of hydrolysis temperatures, enzymolysis time 4h, material-water ratio 20% under the centrifugal 30min condition of 4500r/min, is investigated the influence of pH to fatty acid distribution, the results are shown in Table 2-5.By table 2-5 result as can be seen pH near 9 near saturated fatty acid: monounsaturated fatty acids: polyunsaturated fatty acid=(0-1): 1: 1, near 0.27: 1: 1, n-6 polyunsaturated fatty acid: n-3 polyunsaturated fatty acid=4-6: 1, so pH selects 8-10 in the response surface test design below
Table 2-5 enzyme concentration is to the influence of fatty acid distribution
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
At material-water ratio 20%, 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 2-1.Obviously increase when enzyme concentration total oily extraction yield greater than 1.7% time as can be seen by Fig. 2-1 result, so the enzyme concentration level is selected 1.3-2.1% 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 20%, 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 2-2.By Fig. 2-2 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 20%, 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 2-3.By Fig. 2-3 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 2-4.By Fig. 2-4 result as can be seen material-water ratio obviously increase greater than 15% total oily extraction yield, but when material-water ratio greater than 35%, total oily extraction yield is on a declining curve, so material-water ratio is selected 15%-35% in the response surface test design below.
2.2.5pH influence to total oily extraction yield
At enzyme concentration 2%, 55 ℃ of hydrolysis temperatures, enzymolysis time 4h, material-water ratio 20% 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 2-5.By Fig. 2-5 result as can be seen pH near 9-10, have higher value to occur, so pH selects 8-10 in the response surface test design below.
2.3 the response surface optimum experimental reaction conditions of enzymolysis process
2.3.1 enzymolysis process is to the result that influences of fatty acid distribution
2.3.1.1 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), with monounsaturated fatty acids: the ratio of polyunsaturated fatty acid is response value, according to the center combination principle of design, the experiment of design response surface analysis, its level of factor coding schedule sees Table 2-6.
Table 2-6 level of factor coding schedule
2.3.1.2 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
5Be independent variable(s), with monounsaturated fatty acids: the ratio of polyunsaturated fatty acid is response value Y, response surface experimental program and the results are shown in Table 2-7.Experiment 1-26 is factorial experiment, and 27-36 is 10 center tests, in order to the estimating experiment error.
Table 2-7 response surface experimental program and experimental result
2.3.1.3 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
1=-4.08556+3.295313X
1-0.021729X
2+ 0.893542X
3-0.086229X
4+ 0.504792X
5-0.028646X
1 2-0.006875X
1X
2-0.34375X
1X
3+ 0.008125X
1X
4-0.20625X
1X
5+ 0.000554X
2 2-0.01325X
2X
3+ 0.000675X
2X
4-0.00075X
2X
5-0.024583X
3 2-0.00625X
3X
4+ 0.0825X
3X
5-0.000996X
4 2+ 0.01225X
4X
5-0.034583X
5 2(2-1) regression analysis and The results of analysis of variance see Table 2-8, and the response surface optimizing sees Table 2-9, and Dimension Reduction Analysis is seen Fig. 2-6, and significant mutually alternately response surface analysis is seen Fig. 2-7.
Table 2-8 returns and The results of analysis of variance
By showing 2-8 as can be known, 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=92.58%, R
2 Adj=82.68%, 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＞x
5, i.e. solid-liquid ratio＞enzyme concentration＞enzymolysis time＞hydrolysis temperature＞pH.
Application responds face optimizing analytical procedure is analyzed regression model, seeks optimal response and the results are shown in Table 2-9, and working as enzyme concentration as can be known by table 2-9 is 2.12%, temperature is 50 ℃, and enzymolysis time is 2.8h, and material-water ratio is 39%, pH is 10.5, and response surface has optimum value 1.01 ± 0.02.
Table 2-9 response surface optimizing result
By each enzymolysis parameter of Fig. 2-6 as can be known, along with monounsaturated fatty acids in the increase grease of enzyme concentration is more than polyunsaturated fatty acid to the Dimension Reduction Analysis of fatty acid distribution influence; Monounsaturated fatty acids under the certain temperature condition: it is more than polyunsaturated fatty acid that polyunsaturated fatty acid approaches under 1 other temperature condition in the grease monounsaturated fatty acids, approaches 1 at 50 ℃ of left and right sides ratios; Time is little to the fatty acid distribution influence, and along with the increase of enzymolysis time, polyunsaturated fatty acid also increases to some extent, and its ratio is remained on about 1; Solid-liquid ratio can keep monounsaturated fatty acids within the specific limits: polyunsaturated fatty acid approaches 1, remains on about 40 best; The polyunsaturated fatty acid that increases in the oil along with ph increases, and is optimum ph in about 10.5.
Can find out by Fig. 2-7 analytical results: enzyme concentration (x
1) and enzymolysis time (x
3), hydrolysis temperature (x
2) and enzymolysis time (x
3), hydrolysis temperature (x
2) and solid-liquid ratio (x
4), hydrolysis temperature (x
2) and enzymolysis pH value (x
5) interaction to the influence of fatty acid distribution.Hence one can see that in enzymolysis ph is the 10-11 scope, though enzymolysis ph is minimum to the factor contributions rate of fatty acid distribution, the interaction of hydrolysis temperature and other factors is bigger to the fatty acid distribution influence.
2.3.2 enzymolysis process is to the result that influences of total oil extracting rate
2.3.2.1 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 2-10
Table 2-10 level code table
2.3.2.2 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
2Response surface experimental program and to the results are shown in Table 2-11 experiment 1-26 be factorial experiment, 27-36 is 10 centers tests, in order to the estimating experiment error.
Table 2-11 response surface experimental program and experimental result
2.3.2.3 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=-302.572+145.4542X
1+ 3.076333X
2+ 73.62167X
3-3.877167X
4+ 23.96208X
5-8.541667X
1 2-0.57X
1X
2-18.9X
1X
3+ 0.575X
1X
4-4.1375X
1X
5-0.026567X
2 2-0.203X
2X
3+ 0.0091X
2X
4+ 0.1435X
2X
5-2.206667X
3 2+ 0.093X
3X
4-1.975X
3X
5-0.014367X
4 2+ 0.3215X
4X
5-1.421667X
5 2(2-2) regression analysis and The results of analysis of variance see Table 2-12, and the response surface optimizing sees Table 2-13, and Dimension Reduction Analysis is seen Fig. 2-10, and significant mutually alternately response surface analysis is seen Fig. 2-11
Table 2-12 returns and The results of analysis of variance
By showing 2-12 as can be known, 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=96.65%, R
2 Adj=92.18%, 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
1＞x
3＞x
5＞x
2＞x
4, i.e. enzyme concentration＞hydrolysis temperature＞pH＞enzymolysis time＞solid-liquid ratio.
Application responds face optimizing analytical procedure is analyzed regression model, seeks optimal response and the results are shown in Table 2-13, and working as enzyme concentration as can be known by table 2-13 is 1.84%, temperature is 50 ℃, and enzymolysis time is 3.3h, and material-water ratio is 17.6, pH is 8, and response surface has optimum value 91.93 ± 0.5%.
Table 2-13 response surface optimizing result
Total by each enzymolysis parameter of Fig. 2-6 to the Dimension Reduction Analysis of oily extraction yield as can be known, total oily extraction yield increases with the increase of enzyme concentration, but the trend that the later stage increases is not obvious, continues to increase enzyme concentration and can increase production cost.Total oily extraction yield changes little with hydrolysis temperature, this is main because Sumizyme MP hydrolysis result under alkaline condition is all better, total oily extraction yield is subjected to the influence of hydrolysis temperature little in more excellent scope.Total oily extraction yield increases with the increase of enzymolysis time, total but after reaching certain hour oily extraction yield will no longer increase.Total oily extraction yield increases with the increase of solid-liquid ratio, continue to increase solid-liquid ratio behind the certain value and can dilute concentration of substrate but reach, so total oily extraction yield reduce.Total oily extraction yield increases afterwards earlier with the increase of enzymolysis pH value and reduces, and is the higher value appearance to be arranged near 8 in the pH value.
Can find out by Fig. 2-7 analytical results: enzyme concentration (x
1) and hydrolysis temperature (x
2), enzyme concentration (x
1) and enzymolysis time (x
3), enzyme concentration (x
1) and solid-liquid ratio (x
4), enzyme concentration (x
1) and enzymolysis pH value (x
5), hydrolysis temperature (x
2) and enzymolysis time (x
3), hydrolysis temperature (x
2) and enzymolysis pH value (x
5), enzymolysis time (x3) and enzymolysis pH value (x
5) and solid-liquid ratio (x
4) and enzymolysis pH value (x
5) interaction to the influence of total oily extraction yield.Solid-liquid ratio is to the factor contributions rate minimum of total oily extraction yield in solid-liquid ratio is the 25%-35% scope though hence one can see that, and the interaction of solid-liquid ratio and other factors is bigger to total oily extraction yield influence.
2.3 the fuzzy evaluation optimization of enzymolysis process parameter
The regression model of respectively being investigated index by above research as can be seen, different investigation indexs are followed different Regression Model.So just caused difficulty to parameters Optimization, after promptly with a certain investigation index technology being optimized, under these processing condition, other investigate index may depart from expected value.This just relates to the multi-objective optimization question of processing parameter.
Multiple-objection optimization is to be a new comprehensive single goal with a plurality of investigation desired values by certain formal transformation, again by the optimization to this simple target, reaches purpose (Chen Min etc., 1995 of multiple-objection optimization indirectly; Woods file cloud, 1992; Kang Lining, 2007).
Common multiple goal integrated evaluating method comprises (woods file cloud etc., 1992 such as composite index law, PCA, factor analysis, entropy method, expert assessment method, fuzzy comprehensive evaluation method, economic analysis method, efficiency coefficient method, multiple goal effectiveness synthetic method, analytical hierarchy process; Su Weihua, 2001; Yu Xiaofen, 2004; Kang Lining, 2007).
This research is used fuzzy comprehensive evaluation method this test main investigation total oily extraction yield of index and fatty acid ratio is carried out two objective optimization, and obtain best enzymolysis process parameter at this problem.
2.3.1 comprehensive evaluation method
High grease extraction yield and balancing fatty-acid ratio to be obtained simultaneously, an index can not be only considered.So by fuzzy comprehensive evaluation method grease extraction yield and fatty acid ratio are carried out multifactorial evaluation, seek relatively reasonably enzymolysis process parameters combination.Here use the frequency analysis to seek best enzymolysis process parameter (Xu Honghua, 2004; Sun Peiling, 2006).
Factor of evaluation collection U={ fatty acid ratio zero dimension conversion values, grease extraction yield zero dimension conversion values }={ U
1, U
2U
1, U
2Funtcional relationship following (testing data sees Table):
U
1(X)＝1-|1-y
2i|、
Respectively orthogonal experiments is brought into and obtain estimating matrix r in the membership function and choose evaluation function and be
R wherein
jBe weight coefficient, i=1,2,3 ..., 36
Take all factors into consideration the significance level (by the evaluation of economic benefit of 20 experts to produce green no solvent residue mixed oil and fatty acid balance nutrition, averaging) of test index, assigning weight is chosen for r={0.67,0.33}.
2.3.2 digital-to-analogue is stuck with paste multifactorial evaluation result's optimization
The response surface optimized method carries out process optimization behind this experimental applications fuzzy comprehensive evoluation.With x
1, x
2, x
3, x
4, x
5Being independent variable(s), is response value D with the fuzzy comprehensive evoluation result, experimental program and the results are shown in Table 2-14.Experiment 1-26 is factorial experiment, and 27-36 is 10 center tests, in order to the estimating experiment error.
Table 2-14 test arrangement and result
Carry out data analysis by statistical analysis software SAS9.1, it is as follows to set up quadratic response face regression model:
D=55347+0.035417X
1+ 0.01875X
2+ 0.032083X
3+ 0.01125X
4+ 0.02625X
5-0.013021X1
2-0.025625X
1X
2-0.054375X
1X
3+ 0.021875X
1X
4-0.008125X
1X
5-0.026771X
2 2-0.020625X
2X
3+ 0.008125X
2X
4+ 0.025625X
2X
5-0.020521X
3 2+ 0.006875X
3X
4-0.018125X
3X
5-0.023021X
4 2+ 0.028125X
4X
5-0.013021X5
2(2-3) recurrence sees Table 2-15 with The results of analysis of variance, and response surface is optimized fuzzy evaluation and be the results are shown in Table 2-16, and Dimension Reduction Analysis is seen Fig. 2-10
Table 2-15 returns and The results of analysis of variance
By showing 2-15 as can be known, 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=95.67%, R
2 Adj=89.89%, 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
1＞x
3＞x
5＞x
2＞x
4, i.e. enzyme concentration＞enzymolysis time＞pH＞hydrolysis temperature＞solid-liquid ratio.
Application responds face method for optimization analysis is analyzed fuzzy evaluation result's regression model, seek optimal response and the results are shown in Table 2-16, working as enzyme concentration as can be known by table 2-16 is 1.88%, temperature is 48 ℃, enzymolysis time is 3.5h, material-water ratio is 22.5, and pH is 8.1, and it is 0.9553 ± 0.018 that response surface is optimized the fuzzy evaluation end value.
Table 2-16 response surface optimizing result
By each enzymolysis parameter of Fig. 2-10 to the Dimension Reduction Analysis comparative study of total oily extraction yield as can be known to the Dimension Reduction Analysis of fuzzy evaluation result's Dimension Reduction Analysis and each enzymolysis parameter fatty acid distribution of Fig. 2-6 and each enzymolysis parameter of Fig. 2-8, therefore each enzymolysis process parameter influences rule to fatty acid distribution, total oily extraction yield and fuzzy evaluation result similarity, utilizes the fuzzy evaluation optimized method to take into account to obtain the enzymolysis process parameter of fatty acid balance and high grease extraction yield.
2.4 confirmatory experiment
Application responds face method for optimization analysis is analyzed fuzzy evaluation result's regression model, searching out the best enzymolysis process parameter of taking into account high grease and protein extracting ratio simultaneously is: enzyme concentration is 1.88%, and temperature is 48 ℃, and enzymolysis time is 3.5h, material-water ratio is 22.5, and pH is 8.1.According to level of factor coding schedule 2-6 and 2-10, with the pairing level value of each factor under these processing condition respectively substitution equation 2-1 and the 2-2 regression equation of trying to achieve predict the outcome and see Table 2-17.
By table 2-17 proof test result as can be known, under the optimum enzymatic hydrolysis condition of the Sumizyme MP that fuzzy evaluation is optimized, the predictor of fatty acid ratio is 1.003,5 times proof test mean value is 1.021, and verified saturated fatty acid: monounsaturated fatty acids: polyunsaturated fatty acid is 0.31: 1.021: 1, the n-6 polyunsaturated fatty acid: the n-3 polyunsaturated fatty acid is to satisfy fatty acid balance at 4.71: 1.Total oily extraction yield predictor is 90.34%, 5 times proof test mean value is 90.08%, found that by above, each investigates the validation value of index and the standard deviation between the predictor all in the reasonable scope, proof test value and regression equation predictor that response value is described are coincide well, and proving by fuzzy evaluation method optimum result has good repeatability.And can be met the mixed oil of fatty acid balance and high oil extracting rate simultaneously, the quality of mixed oil is also very high, has so not only satisfied people's diet balance but also can save production line.
Table 2-17 proof test result
The optimal process parameter of the pulverizing expelling-expansion pretreatment technology of raw material experiment before experimental example 3 enzymolysis
Processing parameter based on the fixed best aqueous enzymatic extraction mixed oil of experimental example 2 carries out single factor squeeze test, determines the scope of each extruding puffing system parameter (sleeve temperature, nib aperture, screw speed, material water rate).With fatty acid ratio and total oil extracting rate 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
What soybean Heilungkiang Academy of Agricultural Sciences cultivated cultivates agricultural 42
Peanut
Linseed oil
The tea seed
Protamex 6L Sumizyme MP 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
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
GC-2010 type gas chromatograph (day island proper Tianjin company)
Multiple oil plant synchronized mixes machine self-control
1.3 experimental technique
1.3.1 technical process
Soybean, peanut, linseed oil, tea seed are mixed in proportion (soybean 49%, peanut 28.5%, linseed oil 14.4%, tea seed 8.1%) → pulverizing → moisture adjusting → extruding puffing → pulverizing → adjusting pH value and temperature → enzymolysis (Alcalase alkaline endo proteolytic enzyme, processing condition are: enzyme concentration is 1.88%, and temperature is 48 ℃, and enzymolysis time is 3h30min, material-water ratio is 22.5%, and pH is 8.1) → enzyme → centrifugation of going out → mixed oil
↓ (residue is collected and is measured the Residual oil quality)
Polypeptide powder ← spraying drying ← hydrolyzed solution, milk sap → breakdown of emulsion → mixed oil
1.3.2 the selection of extruding puffing system parameter
On the former study basis, on the basis of single factor research, determine the level value scope of each factor, adopt response surface central. set and test design, study each extruding puffing parameter to investigating the rule that influences of index.With nib aperture, material water ratio, screw speed, 4 factors of sleeve temperature is independent variable(s), is response value with fatty acid distribution and total oily extraction yield, and its level of factor coding schedule sees Table 3-1.
Table 3-1 level of factor coding schedule
2 results and discussion
2.1 response surface experimental establishment and experimental result
2.1.1 extruding puffing is to the response surface experiment of fatty acid distribution influence
With x
1, x
2, x
3, x
4Be independent variable(s), with monounsaturated fatty acids: the ratio of polyunsaturated fatty acid is response value Y
1Response surface experimental program and the results are shown in Table 3-1.Experiment 1-24 is factorial experiment, and 25-36 is 12 center tests, in order to the estimating experiment error.
Table 3-1 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:
Y
1＝0.652948-0.056559X
1+0.154497X
2-0.003053X
3-0.009252X
4-0.000468X
1 2+0.004299X
1X
2-0.00037X
1X
3+0.00036X
1X
4-0.009152X
2 2+0.000988X
2X
3+0.000099X
2X
4-0.000047X
3 2+0.000012X
3X
4-0.0000006863-6X
4 2(3-1)
Regression analysis and The results of analysis of variance see Table 3-2, and the response surface optimizing the results are shown in Table 3-3, and Dimension Reduction Analysis is seen Fig. 3-1, significant mutually alternately response surface Fig. 3-2
Table 3-2 returns and The results of analysis of variance
By table 3-6 as can be known, 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=90.58%, R
2 Adj=84.30%, 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
2＞x
3＞x
1＞x
4It is material water ratio＞screw speed＞nib aperture＞sleeve temperature.
Table 3-3 response surface optimizing result
By Fig. 3-1 as can be seen each factor to investigating the rule that influences of index fatty acid distribution.Nib aperture, sleeve temperature are to the fatty acid distribution influence not quite, along with the increase polyunsaturated fatty acid of material water ratio is more than the content of monounsaturated fatty acids, water content 20% left and right sides monounsaturated fatty acids and polyunsaturated fatty acid reach balance when reaching certain content, ratio is 1: 1, polyunsaturated fatty acid continues to increase when water content continues to increase, and the speed that the content of monounsaturated fatty acids increases is slowed down.Screw speed influence rule and material water ratio to influence rule the same.Promptly monounsaturated fatty acids and polyunsaturated fatty acid can reach balance when 100r/min.
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 19%, and screw speed is 100r/min, and the sleeve temperature is 85 ℃, and response surface has optimum value 0.9975 ± 0.022.
2.1.2 extruding puffing is to the response surface experiment of total oily extraction yield influence
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
2Response surface experimental program and the results are shown in Table 3-4.Experiment 1-24 is factorial experiment, and 25-36 is 12 center tests, in order to the estimating experiment error.
Table 3-4 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:
Y
2＝40.78116-1.332292X
1+5.949896X-0.638905X
3+1.050583X
4-0.030833X
1 2+0.096875*X1*X2-0.014042X
1X
3+0.029875X
1X
4-0.291771X
2 2+0.034188X
2X
3+0.003563X
2X
4+0.000123X
3 2+0.002888X
3X
4-0.013933X
4 2(3-2)
Regression analysis and The results of analysis of variance see Table 3-5, and the response surface optimizing the results are shown in Table 3-6, and Dimension Reduction Analysis is seen Fig. 3-3, significant mutually alternately response surface Fig. 3-4
Table 3-5 returns and The results of analysis of variance
By table 3-5 as can be known, 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=94.12%, R
2 Adj=90.20%, 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
1＞x
4＞x
2＞x
3It is nib aperture＞sleeve temperature＞material water ratio＞screw speed.
Table 3-6 response surface optimizing result
By Fig. 3-3 as can be seen each factor to investigating the rule that influences of the total oily extraction yield of index.Total oily extraction yield is with nib aperture x
1Increase increase earlier and afterwards change not quite.Total oily extraction yield is with material water ratio x
2Increase increase afterwards earlier and reduce.Total oily extraction yield is with screw speed x
3Increase, successively change little.Total oily 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 24mm, and material water ratio is 21%, and screw speed is 110r/min, and the sleeve temperature is 77 ℃, and response surface has optimum value 92.70 ± 0.57%.
3.3 the fuzzy evaluation optimization of enzymolysis process parameter
The regression model of respectively being investigated index by above research as can be seen, different investigation indexs are followed different Regression Model.So just caused difficulty to parameters Optimization, after promptly with a certain investigation index technology being optimized, under these processing condition, other investigate index may depart from expected value.This just relates to the multi-objective optimization question of processing parameter.
Multiple-objection optimization is to be a new comprehensive single goal with a plurality of investigation desired values by certain formal transformation, again by the optimization to this simple target, reaches purpose (Chen Min etc., 1995 of multiple-objection optimization indirectly; Woods file cloud, 1992; Kang Lining, 2007).
Common multiple goal integrated evaluating method comprises (woods file cloud etc., 1992 such as composite index law, PCA, factor analysis, entropy method, expert assessment method, fuzzy comprehensive evaluation method, economic analysis method, efficiency coefficient method, multiple goal effectiveness synthetic method, analytical hierarchy process; Su Weihua, 2001; Yu Xiaofen, 2004; Kang Lining, 2007).
This research is used fuzzy comprehensive evaluation method this test main investigation total oily extraction yield of index and fatty acid ratio is carried out two objective optimization, and obtain best extruding puffing parameter at this problem.
3.3.1 comprehensive evaluation method
High grease extraction yield and balancing fatty-acid ratio to be obtained simultaneously, an index can not be only considered.So by fuzzy comprehensive evaluation method grease extraction yield and fatty acid ratio are carried out multifactorial evaluation, seek relatively reasonably extruding-puffing technique parameters combination.Here use the frequency analysis to seek best extruding-puffing technique parameter (Xu Honghua, 2004; Sun Peiling, 2006).
Factor of evaluation collection U={ fatty acid ratio zero dimension conversion values, total grease extraction yield zero dimension conversion values }={ U
1, U
2}
U
1, U
2Funtcional relationship following (testing data sees Table):
U
1(X)＝1-/1-y
2i/、
Respectively orthogonal experiments is brought into and obtain estimating matrix r in the membership function and choose evaluation function and be
R wherein
jBe weight coefficient, i=1,2,3 ..., 36
Take all factors into consideration the significance level (by the evaluation of economic benefit of 20 experts to produce green no solvent residue mixed oil and fatty acid balance nutrition, averaging) of test index, assigning weight is chosen for r={0.67,0.33}.
2.3.2 digital-to-analogue is stuck with paste multifactorial evaluation result's optimization
The response surface optimized method carries out process optimization behind this experimental applications fuzzy comprehensive evoluation.With x
1, x
2, x
3, x
4, x
5Being independent variable(s), is response value D with the fuzzy comprehensive evoluation result, experimental program and the results are shown in Table 3-7.Experiment 1-26 is factorial experiment, and 27-36 is 10 center tests, in order to the estimating experiment error.
Table 3-7 test arrangement and result
Carry out data analysis by statistical analysis software SAS9.1, it is as follows to set up quadratic response face regression model:
D＝-7.9525-0.164271X
1+1.350417X
2-0.041667X
3+0.000611X
4-0.000859X
1 2+0.010938X
1X
2-0.000594X
1X
3+0.000708X
1X
4-0.05X
2 2+0.002875X
2X
3+0.000167X
2X
4-0.000024X
3 2+0.000056X
3X
4-0.000156X
4 2(3-3)
Return with The results of analysis of variance and see Table 3-8, response surface is optimized fuzzy evaluation and be the results are shown in Table 3-9, and Dimension Reduction Analysis is seen Fig. 3-5
Table 3-8 returns and The results of analysis of variance
By showing 3-8 as can be known, 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=97.51%, R
2 Adj=95.85%, 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
2＞x
1＞x
3＞x
4, i.e. material water ratio＞nib aperture＞screw speed＞sleeve temperature.
Application responds face method for optimization analysis is analyzed fuzzy evaluation result's regression model, seek optimal response and the results are shown in Table 3-9, working as the nib aperture as can be known by table 3-9 is 22mm, material water ratio is 20%, screw speed is 110r/min, the sleeve temperature is 81 ℃, and response surface has optimum value 0.9391 ± 0.015.
Table 3-9 response surface optimizing result
By each extruding-puffing technique parameter of Fig. 3-5 to the Dimension Reduction Analysis of fatty acid distribution and each enzymolysis parameter of Fig. 3-3 as can be known to the Dimension Reduction Analysis comparative study of total oily extraction yield to fuzzy evaluation result's Dimension Reduction Analysis and each extruding puffing parameter of Fig. 3-1, each extruding-puffing technique parameter influences the rule all similar to fatty acid distribution, total oily extraction yield and fuzzy evaluation result, the extruding-puffing technique parameter of therefore utilizing the fuzzy evaluation optimized method to take into account to obtain fatty acid balance and total oily extraction yield.
2.3.4 confirmatory experiment
Application responds face method for optimization analysis is analyzed fuzzy evaluation result's regression model, searches out the best extruding-puffing technique parameter of taking into account fatty acid balance and high total oily extraction yield simultaneously to be; Nib aperture 22mm, material moisture 20%, screw speed 110r/min, 81 ℃ of sleeve temperature.According to level of factor coding schedule 3-1, with the pairing level value of each factor under these processing condition respectively substitution equation 3-1 and the 3-2 regression equation of trying to achieve predict the outcome and see Table 3-10.
Table 3-10 confirmatory experiment result
By table 3-10 proof test result as can be known, under the optimum enzymatic hydrolysis condition of Sumizyme MP and optimum extruding puffing condition that fuzzy evaluation is optimized, the predictor of fatty acid ratio is 1.01,5 times proof test mean value is 1, and verified saturated fatty acid: monounsaturated fatty acids: polyunsaturated fatty acid is 0.29: 1: 1, the n-6 polyunsaturated fatty acid: the n-3 polyunsaturated fatty acid is to satisfy fatty acid balance at 4.36: 1, total oily extraction yield predictor is 91.41%, 5 times proof test mean value is 91.18%, found that by above, each investigates the validation value of index and the standard deviation between the predictor all in the reasonable scope, proof test value and regression equation predictor that response value is described are coincide well, and proving by fuzzy evaluation method optimum result has good repeatability.With fatty acid ratio and total oily extraction yield serves as that the main index of investigating is carried out the mixed oil that the optimum extruding puffing parameter of fuzzy evaluation optimization can promptly be satisfied fatty acid balance and the high oil extracting rate of high quality.
Claims (3)
1. the soybean mixed oil extracting method of a fatty acid balance is characterized in that this method may further comprise the steps:
(1) soybean and peanut, linseed oil, tea seed are mixed in proportion to such an extent that mix oil plant, the shared per-cent of each composition is by weight: the soybean addition is 49%, peanut addition 28.5%, linseed oil addition 14.4%, tea seed addition 8.1%;
(2) the mixing oil plant that obtains in the above-mentioned steps (1) being pulverized the back handles with the screw extruder extruding puffing, mixing oil plant water content after the pulverizing is adjusted into 18%-22%, the aperture of screw extruder nib is 16-24mm, the screw extruder screw speed is 70-130r/min, and screw extruder sleeve temperature is 65 ℃-95 ℃;
(3) the mixing oil plant after the extruding puffing processing in the step (2) is mixed with water, obtain mixed solution, mixed solution massfraction 15%-25%, the pH value of mixed solution is adjusted to 8-10, add proteolytic enzyme and carry out enzymolysis, by weight percentage, the proteolytic enzyme consumption that is added accounts for the 1.3-2.1% of reaction mixture gross weight, hydrolysis temperature is 45 ℃-65 ℃, and enzymolysis time is 2-6 hour;
(4) introduce go out enzyme and centrifugation and handle finishing mixed solution that enzymolysis obtains in the step (3), promptly get the soybean mixed oil product of fatty acid balance, centrifugal rotational speed is 4500r/min; Centrifugation time is 30min.
2. the soybean mixed oil extracting method of fatty acid balance according to claim 1, it is characterized in that: mixing the oil plant water ratio after preferred the pulverizing is 20%, the aperture of screw extruder nib is 22mm, and the screw extruder screw speed is 110r/min, and screw extruder sleeve temperature is 81 ℃.
3. the soybean mixed oil extracting method of fatty acid balance according to claim 1, it is characterized in that: the mixing oil plant behind the preferred extruding puffing mixes the mixed solution massfraction that obtains with water be 22.5%, the pH value of mixed solution is 8.1, it is 1.88% that the proteolytic enzyme consumption accounts for the mixture total weight amount, hydrolysis temperature is 48 ℃, and enzymolysis time is 3 hours 30 minutes.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102559367A (en) * | 2012-02-27 | 2012-07-11 | 东北农业大学 | Method for extracting sesame oil |
| CN102827684A (en) * | 2012-09-13 | 2012-12-19 | 东北农业大学 | Method for extracting flaxseed fat by using extrusion aqueous enzymic method |
| CN103589502A (en) * | 2013-11-29 | 2014-02-19 | 东北农业大学 | Preparation method for blend oil with balanced fatty acid ratio |
| CN104745288A (en) * | 2015-03-23 | 2015-07-01 | 中南林业科技大学 | Process for extracting black tea oil |
| CN104839352A (en) * | 2015-04-30 | 2015-08-19 | 安庆市顺民粮油贸易有限公司 | Puerpera health-caring edible oil and manufacture method thereof |
| CN104839354A (en) * | 2015-04-30 | 2015-08-19 | 安庆市顺民粮油贸易有限公司 | Elderly health care edible oil and production method thereof |
| CN105462681A (en) * | 2015-12-23 | 2016-04-06 | 刘家容 | Extracting process regulating grease ratio of colza oil |
| CN106922853A (en) * | 2017-04-25 | 2017-07-07 | 广州市金妮宝食用油有限公司 | The ready-mixed oil and its production method of a kind of balanced fatty acid |
| CN108913328A (en) * | 2018-08-04 | 2018-11-30 | 望江县振兴植物油厂（普通合伙） | A kind of preparation process of nutrient blend oil |
| CN110786390A (en) * | 2019-11-25 | 2020-02-14 | 佳格食品(中国)有限公司 | High-stability blend oil with blood fat regulating function and preparation method thereof |
| CN110826025A (en) * | 2019-11-25 | 2020-02-21 | 佳格食品(中国)有限公司 | Method for optimizing performance of blending oil by using response surface method and matrix method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1748540A (en) * | 2005-10-17 | 2006-03-22 | 山西省农业科学院农产品综合利用研究所 | The plant blend oil of nutrient balance |
| CN101278748A (en) * | 2008-05-20 | 2008-10-08 | 刘金虹 | Method for preparing edible walnut oil and degreasing walnut protein milk |
| CN101602979A (en) * | 2009-06-09 | 2009-12-16 | 东北农业大学 | A kind of extracting method of soybean oil |
-
2011
- 2011-05-25 CN CN201110136386A patent/CN102229852B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1748540A (en) * | 2005-10-17 | 2006-03-22 | 山西省农业科学院农产品综合利用研究所 | The plant blend oil of nutrient balance |
| CN101278748A (en) * | 2008-05-20 | 2008-10-08 | 刘金虹 | Method for preparing edible walnut oil and degreasing walnut protein milk |
| CN101602979A (en) * | 2009-06-09 | 2009-12-16 | 东北农业大学 | A kind of extracting method of soybean oil |
Non-Patent Citations (1)
| Title |
|---|
| 《中国油脂》 20081231 王瑛瑶等 水酶法提油技术的应用进展 第24-26页 1-3 第33卷, 第7期 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102559367A (en) * | 2012-02-27 | 2012-07-11 | 东北农业大学 | Method for extracting sesame oil |
| CN102827684A (en) * | 2012-09-13 | 2012-12-19 | 东北农业大学 | Method for extracting flaxseed fat by using extrusion aqueous enzymic method |
| CN103589502A (en) * | 2013-11-29 | 2014-02-19 | 东北农业大学 | Preparation method for blend oil with balanced fatty acid ratio |
| CN103589502B (en) * | 2013-11-29 | 2015-04-15 | 东北农业大学 | Preparation method for blend oil with balanced fatty acid ratio |
| CN104745288A (en) * | 2015-03-23 | 2015-07-01 | 中南林业科技大学 | Process for extracting black tea oil |
| CN104839352A (en) * | 2015-04-30 | 2015-08-19 | 安庆市顺民粮油贸易有限公司 | Puerpera health-caring edible oil and manufacture method thereof |
| CN104839354A (en) * | 2015-04-30 | 2015-08-19 | 安庆市顺民粮油贸易有限公司 | Elderly health care edible oil and production method thereof |
| CN105462681A (en) * | 2015-12-23 | 2016-04-06 | 刘家容 | Extracting process regulating grease ratio of colza oil |
| CN106922853A (en) * | 2017-04-25 | 2017-07-07 | 广州市金妮宝食用油有限公司 | The ready-mixed oil and its production method of a kind of balanced fatty acid |
| CN108913328A (en) * | 2018-08-04 | 2018-11-30 | 望江县振兴植物油厂（普通合伙） | A kind of preparation process of nutrient blend oil |
| CN110786390A (en) * | 2019-11-25 | 2020-02-14 | 佳格食品(中国)有限公司 | High-stability blend oil with blood fat regulating function and preparation method thereof |
| CN110826025A (en) * | 2019-11-25 | 2020-02-21 | 佳格食品(中国)有限公司 | Method for optimizing performance of blending oil by using response surface method and matrix method |
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