CN104987947A - Aqueous enzymatic method for soybean fat extraction through isoelectric point demulsification - Google Patents
Aqueous enzymatic method for soybean fat extraction through isoelectric point demulsification Download PDFInfo
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Abstract
The invention relates to an aqueous enzymatic method for soybean fat extraction through isoelectric point demulsification. The method comprises the following steps: crushing soybeans, extruding, crushing, screening, and adding water for mixing; adding basic protease (Protex 6L), and performing enzymolysis; centrifuging a mixed solution after enzymolysis, performing demulsification, and collecting demulsified oil and free oil together. As the emulsion contains lots of discretely distributed oil bodies serving as the main storage parts of fat, the oil bodies are positioned in the same protein net, and protein plays a role of maintaining the oil body stability, the protein structure can be destroyed to release the fat through isoelectric point demulsification. The method is simple in process and equipment, short in demulsification time and high in demulsification rate.
Description
Technical field
The invention belongs to the extraction processing technology of Vegetable oil lipoprotein, relate generally to a kind of method of aqueous enzymatic extraction soybean oil iso-electric point breakdown of emulsion.
Background technology
In the research process of emulsion breakdown, Chinese scholars adopts physics, chemistry, biological method to carry out breakdown of emulsion to milk sap respectively.Li Yang carries out breakdown of emulsion by ultrasonic assistant ethanol procedure, and optimize and obtain best breakdown of emulsion parameter, now free oil extraction rate reached is to (92.60 ± 3.40) %.And the impact that the microstructure change of ultrasonic assistant ethanol breakdown of emulsion discharges its grease by scanning electron microscopic observation, break, so contribute to the release of grease because of the microtexture dispersion of the milk sap of ultrasonic assistant ethanol breakdown of emulsion.Wang Yingyao have studied the test of peanut emulsion breakdown, because peanut milk sap has elasticity, can carry out breakdown of emulsion by raised temperature, increase shearing rate.Because in emulsion interfaces, protein hydrophobic interaction is extremely strong, and the random coil structural content of protein is high on interface, following result is obtained: have selected the freeze-thaw method best to peanut Demulsification of Emulsions by test, freezing, thaw point is respectively-16 DEG C, 35 DEG C, freezing, thawing time is 15h, 2h, and demulsification efficiency is 92.16%.Shaobing Zhang etc. studies the breakdown of emulsion of peanut, and test shows that the most effective breakdown of emulsion means use Sumizyme MP, optimal conditions: the ratio of milk sap and water is 1:1, the addition of enzyme is 1600IU/g, breakdown of emulsion temperature 50 C, breakdown of emulsion time 70min, oil recovery rate reaches 94%.
Lamsal etc. study each component after enzymolysis and are undertaken being separated by separating funnel and the breakdown of emulsion situation of milk sap, carry out emulsion breakdown, and then describe Phospholipid hydrolase in detail to the excision function of each fat key key mapping to the effect of breakdown of emulsion by phospholipase A1, A2, C.J.Wu etc. have inquired into the breakdown of emulsion of soybean emulsion, by comparing the demulsification of Phospholipase A2 and 51FP, reach a conclusion: demulsification is apparently higher than Phospholipase A2 when comparatively few additive for 51FP, and demulsification efficiency can reach 88%.Chabrand etc. also study emulsion breakdown, show that proteolytic enzyme, Phospholipid hydrolase and milk sap acidifying (pH4.5) have remarkable effect to breakdown of emulsion by test, carry out separately the demulsification efficiency that milk sap acidifying (pH4.5) can reach 83%, use a kind of alkaline endo enzyme can reach the demulsification efficiency of 95%, adopt phospholipase A1 and milk sap acidifying associating, the demulsification efficiency of 100% can be reached.Etc. J.M.L.N. proceed the pilot plant test of aqueous enzymatic extraction soybean oil, extracted by two benches, one-phase breakdown of emulsion completes circulation enzymolysis leaching process, improve grease extraction efficiency to 98%, demulsification efficiency reaches 91.60%, and this process reduces the use of water, and carries out cyclophorase solution.
In aqueous enzymatic extraction soybean oil process, breakdown of emulsion problem is a key difficult problem, and the research of breakdown of emulsion in the past all can not be advantageously applied in suitability for industrialized production, and because ethanol is inflammable and explosive, zymin expensive etc., so be all unfavorable for Industry Promotion.Therefore, for the problems referred to above, this experimental study isoelectric point method breakdown of emulsion, efficiently solves breakdown of emulsion problem.
Summary of the invention
Technical problem to be solved by this invention overcomes above-mentioned the deficiencies in the prior art, provides a kind of method of aqueous enzymatic extraction soybean oil iso-electric point breakdown of emulsion, reaches the object simplifying demulsification technology, improve demulsification efficiency.
Technical problem to be solved by this invention is achieved through the following technical solutions:
A kind of method of aqueous enzymatic extraction soybean oil iso-electric point breakdown of emulsion, the method comprises the following steps: the full-fat bean sheet of decortication is pulverized by (1), then in extruder, extruding puffing is carried out, pulverize through pulverizer again, sieved by sieving machine, obtain material, material adds water and is mixed to get mixed solution; Regulate pH of mixed with 2N sodium hydroxide, then add the Protex 6L of quality of material 2.5%, make temperature remain on 55 DEG C, 3h is carried out in reaction; After enzymolysis, mixed solution is centrifugal at ultra-high speed refrigerated centrifuge; After centrifugal, the free oil of the superiors is extracted, then milk sap is collected, put into 4 DEG C of refrigerators and preserve, and then carry out breakdown of emulsion, together with breakdown of emulsion oil is collected with free oil; (2) milk sap is taken out a part, adding dilute hydrochloric acid regulates pH to soybean iso-electric point 4.5, then stir, pH is kept to remain at 4.5, and by thermometer control temperature, and recording reacting time, can repeatedly carry out above-mentioned breakdown of emulsion process, finally by centrifugal for above-mentioned mixed solution, obtain breakdown of emulsion oil.
Described breakdown of emulsion temperature is 50-70 DEG C, breakdown of emulsion time 20-40min, breakdown of emulsion number of times 1-4 time.
The optimized parameter of described iso-electric point breakdown of emulsion: breakdown of emulsion temperature 62.77 DEG C, breakdown of emulsion time 34.26min, breakdown of emulsion number of times 2.71.
Advantageous effect of the present invention is as follows:
Because the oil body containing many discrete distribution in milk sap, oil body is the major storage position of grease, and oil body is distributed in an albumen network, albumen plays the stabilization maintaining oil body, by isoelectric point method breakdown of emulsion, can, by the structure deteriorate of albumen, grease be discharged.And this method processing unit is simple, the breakdown of emulsion time is short, demulsification efficiency is high.
Accompanying drawing explanation
Fig. 1 is overall process route figure of the present invention;
Fig. 2 is the effect diagram of breakdown of emulsion number of times to demulsification efficiency;
Fig. 3 is the effect diagram of breakdown of emulsion temperature to demulsification efficiency;
Fig. 4 is the effect diagram of breakdown of emulsion time to demulsification efficiency;
Fig. 5 is breakdown of emulsion temperature and breakdown of emulsion time interaction response surface figure;
Fig. 6 is breakdown of emulsion temperature and breakdown of emulsion number of times interaction response surface figure;
Fig. 7 is breakdown of emulsion time and breakdown of emulsion number of times interaction response surface figure.
Specific embodiments
Below in conjunction with accompanying drawing, the specific embodiment of the invention is described in detail.
Embodiment 1
A kind of method of aqueous enzymatic extraction soybean oil iso-electric point breakdown of emulsion, the method comprises the following steps: the full-fat bean sheet of decortication is pulverized by (1), then in extruder, extruding puffing is carried out, pulverize through pulverizer again, to be sieved to obtain material by sieving machine, sieve 40 order, material adds water and is mixed to get mixed solution, wherein the mass ratio 1:6 of material and water.Regulate pH of mixed to pH9.5 with 2N sodium hydroxide, in mixed solution, then add Sumizyme MP (Protex 6L), Protex 6L accounts for 2.5% of quality of material, makes temperature remain on 55 DEG C, and 3h is carried out in reaction.After enzymolysis, mixed solution is centrifugal at ultra-high speed refrigerated centrifuge, centrifugal speed 9000r/min, temperature 4 DEG C.After centrifugal, the free oil of the superiors is extracted, then milk sap is collected, put into 4 DEG C of refrigerators and preserve, and then carry out breakdown of emulsion, together with breakdown of emulsion oil is collected with free oil.(2) milk sap is taken out, add 2N dilute hydrochloric acid and regulate pH to soybean iso-electric point 4.5, then stir, pH is kept to remain at 4.5, and by thermometer control temperature, and recording reacting time, can repeatedly carry out above-mentioned breakdown of emulsion process, finally by centrifugal for above-mentioned mixed solution, obtain breakdown of emulsion oil.Breakdown of emulsion temperature 62.77 DEG C, breakdown of emulsion time 34.26min, breakdown of emulsion number of times 2.71.
Embodiment 2
Above-mentioned breakdown of emulsion temperature is 50 DEG C, breakdown of emulsion time 40min, breakdown of emulsion number of times 1 time.Other steps are with embodiment 1.
Embodiment 3
Above-mentioned breakdown of emulsion temperature is 70 DEG C, breakdown of emulsion time 20min, breakdown of emulsion number of times 4 times; Other steps are with embodiment 1.
Embodiment 4
In described step 1, the mass ratio 3:10 of material and water; The Protex 6L added accounts for 5% of amount; Hydrolysis temperature remains on 70 DEG C, and enzyme digestion reaction carries out 2h; Milk sap is collected and is put into 1 DEG C of refrigerator preservation; In described step 2, stating breakdown of emulsion temperature is 60 DEG C, breakdown of emulsion time 30min, breakdown of emulsion number of times 2 times; Other steps are with embodiment 1.
Embodiment 5
In described step 1, the mass ratio 1:4 of material and water; The Protex 6L added accounts for 4% of quality of material; Hydrolysis temperature remains on 60 DEG C, and enzyme digestion reaction carries out 4h; Milk sap is collected and is put into 7 DEG C of refrigerators preservations; Other steps are with embodiment 1.
Iso-electric point demulsification technology optimized parameter shaker test
1, materials and methods
1.1, test raw material
Soybean, Jilin Feng Zheng Food Co., Ltd; Protex 6L Sumizyme MP, Novozymes Company; Sodium hydroxide, hydrochloric acid, Di Bo chemical inc, Tianjin.
1.1.1 test apparatus and equipment
PHS-3C type acidometer, Shanghai Lei Ci instrument plant; 10L vacuum reaction still, high speed freezing centrifuge, Zhengzhou Greatwall Scientific Industrial & Trading Co., Ltd..
1.2 test method
1.2.1 the mensuration of demulsification efficiency
Milk sap oil length measures by AOAC995.19 method
2 test-results and discussion
2.1 breakdown of emulsion number of times are on the impact of demulsification efficiency
The impact of breakdown of emulsion number of times on demulsification efficiency first increases then to remain unchanged as seen from Figure 2, and breakdown of emulsion number of times is 2 times time, and demulsification efficiency reaches maximum.When breakdown of emulsion number of times is lower than 2 times, demulsification efficiency straight line increases; When breakdown of emulsion number of times is higher than 2 times, demulsification efficiency keeps stable.Because breakdown of emulsion number of times is reaching a timing, the grease in milk sap is extracting substantially, does not change so increase breakdown of emulsion number of times demulsification efficiency.So select breakdown of emulsion number of times 1-3 time when response surface optimization.
2.2 breakdown of emulsion temperature are on the impact of demulsification efficiency
As shown in Figure 3, the impact of breakdown of emulsion temperature on demulsification efficiency first increases rear reduction.When breakdown of emulsion temperature 60 C, demulsification efficiency reaches maximum.When breakdown of emulsion temperature is lower than 60 DEG C, demulsification efficiency increases considerably; When breakdown of emulsion temperature is higher than 60 DEG C, breakdown of emulsion take the lead in slowly declining then straight line reduce.So select breakdown of emulsion temperature 55-65 DEG C during response surface optimization.
2.1.3 the breakdown of emulsion time is on the impact of demulsification efficiency
As shown in Figure 4, the impact of breakdown of emulsion time on demulsification efficiency first increases rear reduction.When the breakdown of emulsion time at 30min time, demulsification efficiency reaches maximum.When the breakdown of emulsion time is less than 30min, breakdown of emulsion takes the lead in significantly increasing; Be greater than 30min in the breakdown of emulsion time, demulsification efficiency straight line reduces.So select breakdown of emulsion time 25-35min during response surface optimization.
The response surface experiments optimization of 2.2 iso-electric point demulsification technologies
2.2.1 experimental factor level code table
On the basis of single factor test research, choose breakdown of emulsion number of times, breakdown of emulsion temperature, breakdown of emulsion time 3 factors are independent variable(s), take demulsification efficiency as response value, according to center combination design principle, the test of design response surface analysis, its level of factor coding schedule is in table 1.
2.2.2 the response surface analysis of emulsion breakdown
According to single factor experiment, response phase method is adopted to optimize breakdown of emulsion parameter.With breakdown of emulsion temperature x
1, breakdown of emulsion time x
2, breakdown of emulsion number of times x
3for independent variable(s), demulsification efficiency y is target value, and testing pressure coefficient and target value are as table 2.Carry out 14 groups of factorial tests respectively, 6 group switching centre tests, reduce testing error by assay optimization.
Following equation is obtained by response surface SAS9.13:
Y＝-698.899+17.34176x
1+16.37411x
2-20.48505x
3-0.127728x
1 2-0.06515x
1x
2+0.34125x
1x
3-0.188751x
2 2+0.23925x
2x
3-1.685288x
3 2
It is extremely significant (P<0.0001) that table 3 shows testing pressure coefficient, loses plan item not remarkable.The R of optimization design
2=0.9909>0.8000,
explanation testing error is low, and model is correct.Result proves that this model can mate well and carrys out prediction experiment result with analytical data.
According to test of significance, once item: x
1, x
2; Quadratic term: x
1x
2, x
1x
3, x
2x
3, x
1 2, x
2 2, x
3 2, above-mentioned mention because of prime implicant all on the impact of target value significantly (p<0.05) because there is mutual item, thus because of the impact between prime implicant be compound.Fig. 5 to Fig. 7 represents interactive response surface and level line.Table 3 reacts and is obtained factor contribution ratio by F inspection be: x
2>x
1>x
3(breakdown of emulsion time > breakdown of emulsion temperature > breakdown of emulsion number of times).
The top condition that Responds Surface Methodology obtains is as follows: breakdown of emulsion temperature 62.77 DEG C, breakdown of emulsion time 34.26min, breakdown of emulsion number of times 2.71, demulsification efficiency predictor (98.08 ± 0.62) %.
2.3 proof test
Carry out three parallel tests at optimum conditions, breakdown of emulsion temperature 62.77 DEG C, breakdown of emulsion time 34.26min, breakdown of emulsion number of times 2.71.Three times test-results is respectively: 97.81%, 97.65%, 98.01%.The mean value of three parallel tests is 97.82%, and this illustrates that response value meets regression forecasting value, and model can predict the physical condition of emulsion breakdown.
3 conclusions
This experimental study impact of breakdown of emulsion condition on demulsification efficiency.Adopt isoelectric point method breakdown of emulsion, the top condition that Responds Surface Methodology obtains is as follows: breakdown of emulsion temperature 62.77 DEG C, breakdown of emulsion time 34.26min, breakdown of emulsion number of times 2.71, demulsification efficiency (98.08 ± 0.62) %.
Table 1 response surface experiments level of factor coding schedule
Table 2 response surface experiments scheme and test-results
Table 3 returns and the results of analysis of variance
Claims (4)
1. the method for an aqueous enzymatic extraction soybean oil iso-electric point breakdown of emulsion, it is characterized in that comprising the steps, (1) the full-fat bean sheet of decortication is pulverized, then in extruder, extruding puffing is carried out, pulverize through pulverizer again, to be sieved to obtain material by sieving machine, material adds water and is mixed to get mixed solution; Regulate pH of mixed with 2N sodium hydroxide, in mixed solution, then add Sumizyme MP (Protex 6L), Sumizyme MP (Protex 6L) accounts for the 2.5-5% of quality of material, makes temperature remain on 55-70 DEG C, and 2-4 h is carried out in reaction; After enzymolysis, mixed solution is centrifugal at ultra-high speed refrigerated centrifuge; After centrifugal, the free oil of the superiors is extracted, then milk sap is collected, put into 1-7 DEG C of refrigerator and preserve, and then carry out breakdown of emulsion, together with breakdown of emulsion oil is collected with free oil; (2) milk sap is taken out, add dilute hydrochloric acid and regulate pH to soybean iso-electric point 4.5, then stir, pH is kept to remain at 4.5, and by thermometer control temperature, and recording reacting time, can repeatedly carry out above-mentioned breakdown of emulsion process, finally by centrifugal for above-mentioned mixed solution, obtain breakdown of emulsion oil.
2. the method for a kind of aqueous enzymatic extraction soybean oil iso-electric point breakdown of emulsion according to claim 1, is characterized in that described breakdown of emulsion temperature is 50-70 DEG C, breakdown of emulsion time 20-40 min, breakdown of emulsion number of times 1-4 time.
3. the method for a kind of aqueous enzymatic extraction soybean oil iso-electric point breakdown of emulsion according to claim 2, is characterized in that described breakdown of emulsion temperature 62.77 DEG C, breakdown of emulsion time 34.26 min, breakdown of emulsion number of times 2.71.
4. the method for a kind of aqueous enzymatic extraction soybean oil iso-electric point breakdown of emulsion according to claim 1, is characterized in that in described step 1, the beans material of pulverizing and the mass ratio 1-3:6-10 of water.
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| CN112138430A (en) * | 2020-09-07 | 2020-12-29 | 同济大学 | Magnetic nanorod demulsifier, preparation method thereof and method for treating nanoemulsion by using magnetic nanorod demulsifier |
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| CN101602979A (en) * | 2009-06-09 | 2009-12-16 | 东北农业大学 | A kind of extracting method of soybean oil |
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| CN107142149A (en) * | 2017-04-28 | 2017-09-08 | 蚌埠市九华油脂有限公司 | A kind of processing method for improving soybean oil oil yield |
| CN112138430A (en) * | 2020-09-07 | 2020-12-29 | 同济大学 | Magnetic nanorod demulsifier, preparation method thereof and method for treating nanoemulsion by using magnetic nanorod demulsifier |
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Application publication date: 20151021 |