CN102827687A - Extraction method of soybean oligosaccharides - Google Patents
Extraction method of soybean oligosaccharides Download PDFInfo
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- CN102827687A CN102827687A CN2012103436564A CN201210343656A CN102827687A CN 102827687 A CN102827687 A CN 102827687A CN 2012103436564 A CN2012103436564 A CN 2012103436564A CN 201210343656 A CN201210343656 A CN 201210343656A CN 102827687 A CN102827687 A CN 102827687A
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Abstract
The invention relates to an extraction method of soybean oligosaccharides, and belongs to the technical field of food processing. The method comprises the following steps that (1) soybean is crushed, then, extrusion puffing pretreatment is adopted, puffing materials are obtained, the puffing materials are mixed with water to obtain mixed solution, alkaline protease is added into the mixed solution for enzymolysis, the centrifugal separation is carried out after the enzymolysis to obtain free oily and emulsion solution, hydrolysate and residue; (2) the hydrolysate obtained in the first step is subjected to microwave treatment, the hydrolysate after the microwave treatment is subjected to centrifugal separation, and soybean grease and supernate are obtained; and (3) the supernate obtained through centrifugal separation is subjected to ultrafiltration treatment, and ultrafiltration permeate is sequentially subjected to reverse osmosis, electrodialysis desalination, macroporous adsorption resin decoloring, nanofiltration concentration and spray drying to obtain the soybean oligosaccharides. The method has the advantages that the required process equipment is simple, the cost is low, the recovery rate of the obtained soybean oligosaccharides is high, the quality is good, and the extraction method is suitable for industrial production.
Description
Technical field
The invention belongs to food processing technology field, relate generally to a kind of process for extracting of soybean oligosaccharide.
Background technology
Exist a large amount of soluble soybean oligose in the hydrolyzed solution that aqueous enzymatic extraction soybean oil process forms; Soybean water-soluble sugar has multiple biological activity; It is a kind of natural functional ingredient; It can improve eating quality, processing characteristics and the appearance characteristics of food, can be used in the protein that suppresses in lipid oxidation and the stable acidic beverage, can also be as dispersion agent, emulsifying agent, stablizer, binder in the food; In food, be with a wide range of applications; Therefore the recovery to soybean oligosaccharide in the hydrolyzed solution is the ten minutes critical step, directly has influence on the economic worth of whole technology, and added value and the new development of food that improves soybean prod had very big meaning.
Most scholars is placed on the research emphasis to hydrolyzed solution and reclaims on the protein, and Liu Zhiqiang (2004) cellulase and polygalacturonase act on vegetable seed, and the hydrolyzed solution that obtains is separated rape seed protein with ultrafiltration process, and the rape seed protein yield is 82.3%; Li Yang (2009) adopts aqueous enzymatic method to combine expelling-expansion pretreatment to extract Sunlover 10, and the total protein yield can reach about 94.17%, has improved nearly 15% than the total protein yield of enzymolysis after traditional damp and hot pre-treatment; Jiang Lihua (2010) adopts aqueous enzymatic method, and stripping oil and X 1000 have carried out pilot scale and enlarge and test simultaneously from peanut; Use disc centrifuge that oil-containing hydrolyzed solution secondary disc-type is separated; Obtain peanut X 1000 powder after spray-dried, protein recovery is 78.11%; In addition, the foreign scholar considers the proteic recovery in the hydrolyzed solution, and still from hydrolyzed solution, does not reclaim the method for soybean oligosaccharide.
Summary of the invention
Technical problem to be solved by this invention is the deficiency that overcomes above-mentioned prior art, and a kind of process for extracting of soybean oligosaccharide is provided, and reaches the purpose that reclaims the high quality soy oligose.
Technical problem to be solved by this invention realizes through following technical scheme:
A kind of process for extracting of soybean oligosaccharide; This method may further comprise the steps: (1) soybean is pulverized the back and adopts expelling-expansion pretreatment to obtain expanded material; Expanded material mixed with water obtain mixed solution; In mixed solution, add Sumizyme MP and carry out enzymolysis, spinning obtains free oil, milk sap, hydrolyzed solution and residue behind the enzymolysis; (2) it is 5 that the hydrolyzed solution that step (1) is obtained is regulated pH, and at microwave power 600W, 50 ℃ of following microwave treatment 1min of microwave temperature, the hydrolyzed solution spinning after the microwave treatment obtains soybean oil and supernatant; (3) supernatant that spinning is obtained carries out uf processing, and said ultrafiltration condition is ultrafiltration pressure 0.05-0.25MPa, ultrafiltration time 5-25min, 20-60 ℃ of ultrafiltration temperature and ultrafiltration pH5-9; (4) ultrafiltration sees through liquid and under 45 ℃ of pressure 13Pa, temperature, carries out reverse-osmosis treated after the uf processing; Under voltage 25V, flow 50L/h, carry out electrodialytic desalting; Under 20 ℃, carry out the macroporous adsorbent resin decolouring; Under pressure 0.6MPa, carry out nanofiltration and concentrate, spraying drying promptly obtains soybean oligosaccharide then.
Described ultrafiltration preferred parameter is: ultrafiltration pressure is 0.12MPa, and the ultrafiltration time is 18.3min, and the ultrafiltration temperature is 50 ℃, and ultrafiltration pH is 6.35.
Present method at first adopts microwave treatment to remove soybean oil in the hydrolyzed solution; Adopt technology for recovery soybean oligosaccharide such as combining ultrafiltration r-o-, electrodialysis, macroporous adsorbent resin again; Present method has that required processing unit is simple, cost is low, soybean oligosaccharide recovery height and quality better, is fit to the characteristics of suitability for industrialized production.
Description of drawings
Fig. 1 is an overall process route map of the present invention
Fig. 2 ultrafiltration pressure and ultrafiltration pH are alternately to the response surface of the oligose recovery
Fig. 3 ultrafiltration time and ultrafiltration pH are alternately to the response surface of the oligose recovery
Fig. 4 ultrafiltration temperature and ultrafiltration pH are alternately to the response surface of the oligose recovery
Embodiment
Below in conjunction with accompanying drawing the specific embodiment of the invention is described in detail,
A kind of process for extracting of soybean oligosaccharide; This method may further comprise the steps: (1) soybean is pulverized the back and adopts expelling-expansion pretreatment to obtain expanded material; Expanded material mixed with water obtain mixed solution; In mixed solution, add Sumizyme MP and carry out enzymolysis, spinning obtains free oil, milk sap, hydrolyzed solution and residue behind the enzymolysis; (2) it is 5 that the hydrolyzed solution that step (1) is obtained is regulated pH, and at microwave power 600W, 50 ℃ of following microwave treatment 1min of microwave temperature, the hydrolyzed solution spinning after the microwave treatment obtains soybean oil and supernatant; (3) supernatant that spinning is obtained carries out uf processing, and said ultrafiltration condition is ultrafiltration pressure 0.05-0.25MPa, ultrafiltration time 5-25min, 20-60 ℃ of ultrafiltration temperature and ultrafiltration pH5-9; (4) ultrafiltration sees through liquid and under 45 ℃ of pressure 13Pa, temperature, carries out reverse-osmosis treated after the uf processing; Under voltage 25V, flow 50L/h, carry out electrodialytic desalting; Under 20 ℃, carry out the macroporous adsorbent resin decolouring; Under pressure 0.6MPa, carry out nanofiltration and concentrate, spraying drying promptly obtains soybean oligosaccharide then.
Described ultrafiltration preferred parameter is: ultrafiltration pressure is 0.12MPa, and the ultrafiltration time is 18.3min, and the ultrafiltration temperature is 50 ℃, and ultrafiltration pH is 6.35.
Embodiment: the optimized parameter shaker test of hydrolyzed solution ultrafiltration
1 materials and methods
1.1 material, reagent
| Soybean | Heilungkiang Academy of Agricultural Sciences cultivates cultivates farming 42, and wherein protein content is 41.6%, and fat content is 21.3%, and water ratio is 10.6%, ash content 4.3%. |
| Alcalase alkaline endo proteolytic enzyme | Novo company (1.2 * 10 5U/mL) |
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 | Jintan City, Jiangsu Province high honour instrument Manufacturing Co., Ltd |
| Electric-heated thermostatic water bath | Yuyao City east electric instrument factory |
| The digestion appearance | Shanghai Qianjian Instrument Co., Ltd. |
| Planetary ball mill | Nanda Tianzun Electronics Co., Ltd., Nanjing |
| Soxhlet extractor | Tianjin Glass Instrument Factory |
| Ultra-filtration equipment | Beijing bright forever Medical Instruments factory |
1.3 experimental technique
1.3.1 the composition measurement of soybean
The mensuration of crude protein: GB6432-94 standard method is carried out
The Suo Shi extraction process is measured among the mensuration of crude fat: the GB5512-85
The mensuration of moisture: GB304-87 measures
Determination of ash: GB5009.4-85
1.3.2 technical process
Soybean → pulverizing → moisture adjusting → extruding puffing → pulverizing → adjusting pH value and the temperature → enzymolysis → enzyme that goes out → centrifugal → hydrolyzed solution → microwave treatment → centrifugal → supernatant → ultrafiltration → see through liquid → r-o-→ electrodialytic desalting → macroporous adsorbent resin decolouring → nanofiltration to concentrate → spraying drying → soybean oligosaccharide
2 results and discussion
2.1 empirical factor level code table
On the basis of single factor research; Choosing ultrafiltration pressure, ultrafiltration time, ultrafiltration temperature and 4 factors of ultrafiltration pH is independent variable(s), is response value with the oligose recovery, according to the center combination principle of design; The experiment of design response surface analysis, its level of factor coding schedule is seen table table 2-1.
Table 2-1 level of factor coding schedule
2.2 response surface EE and experimental result
This experimental applications response surface optimized method carries out process optimization.With A, B, C, D is independent variable(s), is response value with oligose recovery R, and response surface experimental program and result see table 2-2.Experiment 1-24 is factorial experiment, and 25-36 is 12 center tests, in order to the estimating experiment error.
Table 2-2 test arrangement and result
2.3 response surface interpretation
Oligose recovery R carries out data analysis through statistical analysis software Design-Expert, and it is following to set up quadratic response face regression model:
R=85.82-0.75A+0.16B+1.80C+1.10D-0.45AB+0.46AC+1.33AD+0.10BC
-0.60BD-1.72CD-1.85A
2-1.41B
2-1.46C
2-0.67D
2
The recurrence of oligose recovery R and The results of analysis of variance are seen table 2-3, and significant mutually alternately response surface analysis is seen Fig. 2-Fig. 4.
The recurrence and the The results of analysis of variance of the table 2-3 oligose recovery
| Variable | Degree of freedom | Sum of squares | All square | The F value | Pr>;F |
| A | 1 | 13.62 | 13.62 | 10.24 | 0.0043 |
| B | 1 | 0.61 | 0.61 | 0.46 | 0.5041 |
| C | 1 | 77.62 | 77.62 | 58.36 | ＜0.0001 |
| D | 1 | 28.95 | 28.95 | 21.77 | 0.0001 |
| AB | 1 | 3.29 | 3.29 | 2.48 | 0.1305 |
| AC | 1 | 3.40 | 3.40 | 2.56 | 0.1246 |
| AD | 1 | 28.25 | 28.25 | 21.24 | 0.0002 |
| BC | 1 | 0.16 | 0.16 | 0.12 | 0.7322 |
| BD | 1 | 5.76 | 5.76 | 4.33 | 0.0498 |
| CD | 1 | 47.47 | 47.47 | 35.70 | ＜0.0001 |
| A 2 | 1 | 109.05 | 109.05 | 82.00 | ＜0.0001 |
| B 2 | 1 | 63.83 | 63.83 | 47.99 | ＜0.0001 |
| C 2 | 1 | 68.19 | 68.19 | 51.28 | ＜0.0001 |
| D 2 | 1 | 14.46 | 14.46 | 10.88 | 0.0034 |
| Return | 14 | 464.68 | 33.19 | 24.96 | ＜0.0001 |
| Residue | 21 | 27.93 | 1.33 | ? | ? |
| Lose and intend | 10 | 6.40 | 0.64 | 0.33 | 0.9554 |
| Error | 11 | 21.53 | 1.96 | ? | ? |
| Summation | 35 | 492.60 | ? | ? | ? |
2-3 can know that the linear relationship between equation dependent variable and the independent variable(s) is obvious by table, and this regression models is (p significantly<0.0001), lose and intend not remarkable (the p > of item; 0.05), and this model R
2=94.33%, R
2 Adj=90.55%, 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: C>D>A>B, i.e. ultrafiltration temperature>ultrafiltration pH>ultrafiltration pressure>the ultrafiltration time.
Application responds face optimizing analytical procedure is analyzed regression model; Searching optimal response ultrafiltration pressure as a result is 0.1175MPa, and the ultrafiltration time is 18.3min, and the ultrafiltration temperature is 50 ℃; Ultrafiltration pH is 6.35, and it is about 86.26% that the response value oligose recovery has optimum value.
2.4 confirmatory experiment and simultaneous test
Under the top condition that the response surface analysis method is tried to achieve, promptly ultrafiltration pressure is 0.1175MPa, and the ultrafiltration time is 18.3min, and the ultrafiltration temperature is 50 ℃, and ultrafiltration pH is 6.35, carries out 3 parallel laboratory tests, and the MV of 3 parallel laboratory test oligose recovery is 87.88%.Experimental value and regression equation predictor that response value is described are identical good.
Claims (2)
1. the process for extracting of a soybean oligosaccharide; This method may further comprise the steps: (1) soybean is pulverized the back and adopts expelling-expansion pretreatment to obtain expanded material; Expanded material mixed with water obtain mixed solution; In mixed solution, add Sumizyme MP and carry out enzymolysis, spinning obtains free oil, milk sap, hydrolyzed solution and residue behind the enzymolysis; It is characterized in that: it is 5 that the hydrolyzed solution that (2) obtain step (1) is regulated pH, and at microwave power 600W, 50 ℃ of following microwave treatment 1min of microwave temperature, the hydrolyzed solution spinning after the microwave treatment obtains soybean oil and supernatant; (3) supernatant that spinning is obtained carries out uf processing, and said ultrafiltration condition is ultrafiltration pressure 0.05-0.25MPa, ultrafiltration time 5-25min, 20-60 ℃ of ultrafiltration temperature and ultrafiltration pH5-9; (4) ultrafiltration sees through liquid and under 45 ℃ of pressure 13Pa, temperature, carries out reverse-osmosis treated after the uf processing; Under voltage 25V, flow 50L/h, carry out electrodialytic desalting; Under 20 ℃, carry out the macroporous adsorbent resin decolouring; Under pressure 0.6MPa, carry out nanofiltration and concentrate, spraying drying promptly obtains soybean oligosaccharide then.
2. the process for extracting of a kind of soybean oligosaccharide according to claim 1, it is characterized in that described ultrafiltration preferred parameter is: ultrafiltration pressure is 0.12MPa, and the ultrafiltration time is 18.3min, and the ultrafiltration temperature is 50 ℃, and ultrafiltration pH is 6.35.
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Cited By (7)
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| CN103585254A (en) * | 2013-11-22 | 2014-02-19 | 东北农业大学 | Method for synchronously extracting soy isoflavone and soy saponine from hydrolysate of aqueous enzymatic method |
| CN103589766A (en) * | 2013-11-22 | 2014-02-19 | 东北农业大学 | Method for simultaneously extracting soybean peptide and soybean oligosaccharide from aqueous phase produced through aqueous enzymatic method |
| CN104543802A (en) * | 2014-12-17 | 2015-04-29 | 方萌 | Method for extracting soybean oligosaccharides from soybeans |
| 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 |
| CN108690707A (en) * | 2018-05-31 | 2018-10-23 | 镇江虎瑞生物科技有限公司 | A kind of method that microwave prepares soybean oil |
| CN109734753A (en) * | 2018-11-27 | 2019-05-10 | 安徽博悦生物科技有限公司 | A kind of extracting method of soyabean oligosaccharides |
| CN111748047A (en) * | 2020-07-29 | 2020-10-09 | 河南科技大学 | Preparation method of dioscorea opposita oligosaccharide |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103585254A (en) * | 2013-11-22 | 2014-02-19 | 东北农业大学 | Method for synchronously extracting soy isoflavone and soy saponine from hydrolysate of aqueous enzymatic method |
| CN103589766A (en) * | 2013-11-22 | 2014-02-19 | 东北农业大学 | Method for simultaneously extracting soybean peptide and soybean oligosaccharide from aqueous phase produced through aqueous enzymatic method |
| CN103589766B (en) * | 2013-11-22 | 2015-12-09 | 东北农业大学 | A kind of method of simultaneous extraction soybean polypeptide and soybean oligosaccharide from aqueous enzymatic method aqueous phase |
| CN104543802A (en) * | 2014-12-17 | 2015-04-29 | 方萌 | Method for extracting soybean oligosaccharides from soybeans |
| 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 |
| CN108690707A (en) * | 2018-05-31 | 2018-10-23 | 镇江虎瑞生物科技有限公司 | A kind of method that microwave prepares soybean oil |
| CN109734753A (en) * | 2018-11-27 | 2019-05-10 | 安徽博悦生物科技有限公司 | A kind of extracting method of soyabean oligosaccharides |
| CN111748047A (en) * | 2020-07-29 | 2020-10-09 | 河南科技大学 | Preparation method of dioscorea opposita oligosaccharide |
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