CN101177460A - Method for extracting water-soluble soybean polysaccharide from soya bean waste and soybean dregs - Google Patents
Method for extracting water-soluble soybean polysaccharide from soya bean waste and soybean dregs Download PDFInfo
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- CN101177460A CN101177460A CNA2007101645460A CN200710164546A CN101177460A CN 101177460 A CN101177460 A CN 101177460A CN A2007101645460 A CNA2007101645460 A CN A2007101645460A CN 200710164546 A CN200710164546 A CN 200710164546A CN 101177460 A CN101177460 A CN 101177460A
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Abstract
The invention discloses a method for extracting water-soluble soybean polysaccharide from bean pulp and bean dregs, which comprises the steps as follows: petroleum ether degreasing, NaOH quadratic deproteinization, polysaccharide extraction with acid or alkali, active carbon decoloration, vaccum concentration, ethanol sedimentation and dryness and other steps. The method adopts the petroleum ether degreasing and the alkali deproteinization steps to implement pretreatment to the bean pulp and bean dregs, firstly most fattiness and protein in the material are removed, and then the water-soluble soybean polysaccharide is extracted by adopting optimized extraction condition, finally the active carbon decoloration and other crafts are implemented on the extractive. The invention has the advantages that: the extraction rate of the water-soluble soybean polysaccharide and the purity of the product can be improved greatly, and the color and lustre of the product is good.
Description
Technical field
The present invention relates to a kind of extraction process of polysaccharide, particularly a kind of method of from dregs of beans, bean dregs, extracting water soluble soybean polysaccharide.
Background technology
Water soluble soybean polysaccharide is the water-soluble polysaccharide that extracts from soybean, because it is higher to contain dietary fiber component, so also be called as the soluble soybean food fibre.Soybean polysaccharide has good physicochemical property, has in the foodstuff additive field very to use widely.
Suspended particles in the water soluble soybean polysaccharide energy stabilize proteins beverage system, its solution viscosity is low, can be used as a kind of very fine stablizer is applied to also can be used as the function raw material of complementary diets fiber in the products such as acidic drinks, whey beverage in the stable suspersion particle; Soybean polysaccharide also can be used as water conservation, guarantor's type and the dispersion agent of various food (fishery products, livestock product, powder food, dessert, the filling heart, Noodles, bread etc.); Because of soybean polysaccharide has certain emulsification effect, it also can be used as the emulsifying agent of products such as beverage, milky-drinks, or as the emulsifying agent and the stablizer of emulsifying property product, as: Emulsion flavour etc.
In the prior art, the extracting method of water soluble soybean polysaccharide adopts mostly and raw material is directly extracted in hot water or extract under acidic conditions, alkaline condition, and extract is generally all without aftertreatment.The reaction conditions of each step is not optimized in these methods, exists extraction yield low, shortcomings such as product purity is low, shade deviation.
Application number is that to disclose a kind of be the method for feedstock production water soluble soybean polysaccharide with dregs of beans, bean dregs for 200610046245.3 Chinese patent application.This method obtains water soluble soybean polysaccharide by adding steps such as water, defibrination, deproteinated, extraction polysaccharide, squeezing, precipitate and separate under certain condition.Extraction yield only is 7%, and this method do not pass through defatting step, and also without suitable aftertreatment, product purity is low, shade deviation for product.
Summary of the invention
A kind of extraction yield height, product purity height, the coloury method of from dregs of beans, bean dregs, extracting water soluble soybean polysaccharide have been the object of the present invention is to provide.
Present method comprises the following steps:
A. degreasing: the dregs of beans, bean dregs and the sherwood oil that are 1: 10～1: 15 by weight drop into the fat extraction device, degreasing reaction 1.0～2.0 hours, and filtration under diminished pressure gets filter cake, and filter cake is in 50～80 ℃ of oven dry down;
B. deproteinated: step a gained filter cake and 13%NaOH (massfraction) solution is 1: 12 mixed by weight, 50 ℃～60 ℃ following water-baths 30～60 minutes, and mixture carries out filtration under diminished pressure;
The gained filter cake carries out the secondary deproteinated with 10%NaOH (massfraction) solution, and the weight ratio of filter cake and NaOH solution is 1: 10,50 ℃～60 ℃ following water-baths 30～60 minutes, and filtration under diminished pressure gets filter cake;
C. extract polysaccharide: add the water of 15～30 times of weight in the step b gained filter cake, regulating pH value with acid is 3～6, or to regulate pH value with alkali be 7.5～12, is heated to 90～120 ℃, reacts 1～2.5 hour, and filtration under diminished pressure gets filtrate;
D. decolouring concentrates: add 0.5～2% gac in the step c gained filtrate, the adjusting pH value is 3～6,40～80 ℃ of water bath heat preservations 15～60 minutes, and centrifugation gets supernatant liquor, and in 45～70 ℃ of following vacuum concentration, the concentrated solution pH value transfers to 6.5-7.5;
E. alcohol precipitation drying: add 95% ethanol in steps d gained concentrated solution, the precipitate and separate polyoses extract washs the back in 50 ℃ of vacuum-dryings with 95% ethanol, dehydrated alcohol, acetone, ether to extract successively, must the water soluble soybean polysaccharide crude product.
Preferably, among the inventive method step a, dregs of beans, bean dregs and sherwood oil weight ratio are 1: 10;
In filter cake, add the water that is equivalent to 20 times of filter cake quality among the step c;
Extracting the used acid of water soluble soybean polysaccharide among the step c can be hydrochloric acid, phosphoric acid, sulfuric acid, lactic acid, citric acid or oxalic acid etc., and used alkali can be sodium hydroxide, potassium hydroxide, yellow soda ash or sodium bicarbonate etc.When using acid extraction, preferred pH value is 3, and temperature is 120 ℃; When using alkaline extraction, preferred pH value is 11, and temperature of reaction is 120 ℃.
The add-on of gac is 1% in the steps d; Regulate concentrated solution pH value to 7.0.
The inventive method adopts petroleum ether degreasing and alkaline solution deproteinated that dregs of beans, bean dregs are carried out pre-treatment, at first remove most of fat and protein in the raw material, adopt the extraction conditions of optimizing to extract water soluble soybean polysaccharide again, at last extract is carried out technologies such as activated carbon decolorizing, improved the purity of the extraction yield and the product of water soluble soybean polysaccharide greatly, and product color is good.
Embodiment
Embodiment 1
Take by weighing 100 gram bean dregs, add 1500 gram sherwood oils, extract 1 hour in Soxhlet fat extraction device, filtration under diminished pressure gets filter cake, in 60 ℃ of bakings 1 hour down, weigh 95 grams.
The gained filter cake mixes with 1140 gram 13%NaOH (massfraction) solution, constantly stirs in 50 ℃ of water-baths and extracts 45 minutes, and filtration under diminished pressure gets filter cake 125g; Filter cake is carried out the secondary deproteinated, and the concentration of sodium hydroxide solution is 10% (massfraction) during the secondary deproteinated, and consumption is 1250 grams, and extraction time is 30 minutes, and filtration under diminished pressure gets filter cake 150 grams.
Up adding 1500mL water in the step gained filter cake, is 4 with the salt acid for adjusting pH value, is heated to 80 ℃, and the reaction times is 60 minutes, and filtration under diminished pressure gets filtrate 1480mL.
Add 8 gram gacs in the above-mentioned filtrate and decolour, regulate pH value to 7.0, bleaching temperature is 60 ℃, bleaching time 15 minutes.Centrifugation goes out supernatant liquor, concentrates with the vacuum concentration method down in 65 ℃.
Regulating the concentrated solution pH value is 7.0, add 95% ethanol, make in the final solution alcoholic acid content more than 80%, precipitation separation obtains polyoses extract, wash with 95% ethanol, dehydrated alcohol, acetone, ether successively, remove impurity, vacuum-drying promptly gets soybean polysaccharide finished product 5.02 grams under 50 ℃ of temperature at last.
Utilize above condition to extract water soluble soybean polysaccharide, yield is 5.02%, and thus obtained water soluble soybean polysaccharide is deep yellow.
Embodiment 2
Take by weighing 100 gram dregs of beans, add 1000 gram sherwood oils, extracted in Soxhlet fat extraction device 1 hour, filtration under diminished pressure gets filter cake, in 60 ℃ of bakings 1 hour, weigh 100 grams.
The gained filter cake mixes with 1200 gram 13%NaOH (massfraction) solution, constantly stirs in 60 ℃ of water-baths and extracts 45 minutes, and filtration under diminished pressure gets filter cake 1 30 grams; Filter cake is carried out the secondary deproteinated, and the concentration of sodium hydroxide solution is 10% (massfraction) during the secondary deproteinated, and consumption is 1300 grams, and extraction time is 30 minutes, and filtration under diminished pressure gets filter cake 160 grams.
Up add 3000ml water in the step gained filter cake, regulating pH value with hydrochloric acid is 3, is heated to 120 ℃, and the reaction times is 90 minutes, and filtration under diminished pressure gets filtrate 2860ml.
Add 29 gram gacs in the above-mentioned filtrate and decolour, regulate pH value to 7.0, bleaching temperature is 80 ℃, bleaching time 30 minutes, and centrifugation goes out supernatant liquor, concentrates with the vacuum concentration method down in 65 ℃.
It is 7.0 that concentrated solution is neutralized to pH value, add 95% ethanol, make in the final solution alcoholic acid content more than 80%, precipitation separation obtains polyoses extract, wash with 95% ethanol, dehydrated alcohol, acetone, ether successively, remove impurity, vacuum-drying promptly gets white soybean polysaccharide crude product 17.56 grams under 50 ℃ of temperature at last.
Utilize above condition to extract water soluble soybean polysaccharide, yield is 17.56%, and thus obtained water soluble soybean polysaccharide is beige.
Embodiment 3
Take by weighing 100 gram dregs of beans, add 1500 gram sherwood oils, extracted 1 hour in Soxhlet fat extraction device, filtration under diminished pressure gets filter cake, in 60 ℃ of bakings 1 hour, is weighed as 95 grams.
The gained filter cake mixes with 1140 gram 13%NaOH (massfraction) solution, constantly stirs in 60 ℃ of water-baths and extracts 45 minutes, and filtration under diminished pressure gets filter cake 125 grams; Filter cake is carried out the secondary deproteinated, and the concentration of sodium hydroxide solution is 10% (massfraction) during the secondary deproteinated, and consumption is 1250 grams, and extraction time is 30 minutes, and filtration under diminished pressure gets filter cake 150 grams.
Up add 1500mL water in the step gained filter cake, regulating pH value with hydrochloric acid is 8, is heated to 60 ℃, and the reaction times is 90 minutes, and filtration under diminished pressure gets filtrate 1480ml.
Add 15 gram gacs in the above-mentioned filtrate and decolour, regulate pH value to 7.0, bleaching temperature is 80 ℃, bleaching time 30 minutes, and centrifugation goes out supernatant liquor, concentrates with the vacuum concentration method down in 65 ℃.
It is 7.0 that concentrated solution is neutralized to pH value, add 95% ethanol, make in the final solution alcoholic acid content more than 80%, precipitation separation obtains polyoses extract, wash with 95% ethanol, dehydrated alcohol, acetone, ether successively, remove impurity, vacuum-drying promptly gets white soybean polysaccharide crude product 6.93 grams under 50 ℃ of temperature at last.
Utilize above condition to extract water soluble soybean polysaccharide, yield is 6.93%, and thus obtained water soluble soybean polysaccharide is beige.
Embodiment 4
Take by weighing 100 gram dregs of beans, add 1200 gram sherwood oils, extracted 1 hour in Soxhlet fat extraction device, filtration under diminished pressure gets filter cake, in 60 ℃ of bakings 1 hour, is weighed as 100 grams.
The gained filter cake mixes with 1200 gram 13%NaOH (massfraction) solution, constantly stirs in 60 ℃ of water-baths and extracts 45 minutes, and filtration under diminished pressure gets filter cake 130 grams; Filter cake is carried out the secondary deproteinated, and the concentration of sodium hydroxide solution is 10% (massfraction) during the secondary deproteinated, and consumption is 1300 grams, and extraction time is 30 minutes, and filtration under diminished pressure gets filter cake 160 grams.
Up add 2000mL water in the step gained filter cake, regulating pH value with hydrochloric acid is 11, is heated to 120 ℃, and the reaction times is 120 minutes, and filtration under diminished pressure gets filtrate 1900ml.
Add 20 gram gacs in the above-mentioned filtrate and decolour, regulate pH value to 4.0, bleaching temperature is 80 ℃, bleaching time 30 minutes, and centrifugation goes out supernatant liquor, concentrates with the vacuum concentration method down in 65 ℃.
It is 7.0 that concentrated solution is neutralized to pH value, add 95% ethanol, make in the final solution alcoholic acid content more than 80%, precipitation separation obtains polyoses extract, wash with 95% ethanol, dehydrated alcohol, acetone, ether successively, remove impurity, vacuum-drying promptly gets white soybean polysaccharide crude product 16.85 grams under 50 ℃ of temperature at last.
Utilize above condition to extract water soluble soybean polysaccharide, yield is 16.85%, and thus obtained water soluble soybean polysaccharide is light beige.
Those of ordinary skill in the art will be appreciated that, above embodiment is used for illustrating the present invention, and be not as limitation of the invention, as long as in essential scope of the present invention, all will drop in the scope of claims of the present invention variation, the modification of the above embodiment.
Claims (8)
1. a method of extracting water soluble soybean polysaccharide from dregs of beans, bean dregs is characterized in that, comprises the following steps:
A. degreasing: the dregs of beans, bean dregs and the sherwood oil that are 1: 10～1: 15 by weight drop into the fat extraction device, degreasing reaction 1.0～2.0 hours, and filtration under diminished pressure gets filter cake, and filter cake is in 50～80 ℃ of oven dry down;
B. deproteinated: step a gained filter cake and 13%NaOH (massfraction) solution is 1: 12 mixed by weight, 50 ℃～60 ℃ following water-baths 30～60 minutes, and mixture carries out filtration under diminished pressure;
The gained filter cake carries out the secondary deproteinated with 10%NaOH (massfraction) solution, and the weight ratio of filter cake and NaOH solution is 1: 10,50 ℃～60 ℃ following water-baths 30～60 minutes, and filtration under diminished pressure gets filter cake;
C. extract polysaccharide: add the water of 15～30 times of weight in the step b gained filter cake, regulating pH value with acid is 3～6, or to regulate pH value with alkali be 7.5～12, is heated to 90～120 ℃, reacts 1～2.5 hour, and filtration under diminished pressure gets filtrate;
D. decolouring concentrates: add 0.5～2% gac in the step c gained filtrate, the adjusting pH value is 3～6,40～80 ℃ of water bath heat preservations 15～60 minutes, and centrifugation gets supernatant liquor, and in 45～70 ℃ of following vacuum concentration, the concentrated solution pH value transfers to 6.5-7.5;
E. alcohol precipitation drying: add 95% ethanol in steps d gained concentrated solution, the precipitate and separate polyoses extract washs the back in 50 ℃ of vacuum-dryings with 95% ethanol, dehydrated alcohol, acetone, ether to extract successively, must the water soluble soybean polysaccharide crude product.
2. the method for extracting water soluble soybean polysaccharide from dregs of beans, bean dregs as claimed in claim 1 is characterized in that among the step a that dregs of beans, bean dregs and sherwood oil mass ratio are 1: 10.
3. the method for extracting water soluble soybean polysaccharide from dregs of beans, bean dregs as claimed in claim 1 is characterized in that among the step c water of 20 times of in filter cake addings.
4. the method for extracting water soluble soybean polysaccharide from dregs of beans, bean dregs as claimed in claim 1 is characterized in that regulating pH value with acid among the step c is 3, and temperature of reaction is 120 ℃.
5. the method for extracting water soluble soybean polysaccharide from dregs of beans, bean dregs as claimed in claim 1 is characterized in that regulating pH value with alkali among the step c is 11, and temperature of reaction is 120 ℃.
6. the method for extracting water soluble soybean polysaccharide from dregs of beans, bean dregs as claimed in claim 1, the add-on that it is characterized in that gac in the steps d is 1%.
7. the method for extracting water soluble soybean polysaccharide from dregs of beans, bean dregs as claimed in claim 1 is characterized in that regulating in the steps d concentrated solution pH value to 7.0.
8. the method for extracting water soluble soybean polysaccharide from dregs of beans, bean dregs as claimed in claim 1,95% alcoholic acid add-on should make that amount of alcohol reaches more than 80% in the final solution when it is characterized in that step e alcohol precipitation.
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| CN101712715A (en) * | 2009-12-18 | 2010-05-26 | 周鑫 | Method for decolorizing full water-soluble soybean glycoprotein |
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| CN102304189A (en) * | 2011-07-20 | 2012-01-04 | 中国农业科学院农产品加工研究所 | Method for extracting anti-oxidant mung bean polysaccharide |
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| CN101712715A (en) * | 2009-12-18 | 2010-05-26 | 周鑫 | Method for decolorizing full water-soluble soybean glycoprotein |
| CN102304189A (en) * | 2011-07-20 | 2012-01-04 | 中国农业科学院农产品加工研究所 | Method for extracting anti-oxidant mung bean polysaccharide |
| CN102558378B (en) * | 2012-01-11 | 2013-12-25 | 上海理工大学 | Preparation method of water-soluble soybean polysaccharide |
| CN102558378A (en) * | 2012-01-11 | 2012-07-11 | 上海理工大学 | Preparation method of water-soluble soybean polysaccharide |
| CN102558381B (en) * | 2012-02-16 | 2013-11-06 | 上海理工大学 | Method for extracting water-soluble soybean polysaccharide from low-temperature bean pulp through microwave-ultrasonic synergism |
| CN102558381A (en) * | 2012-02-16 | 2012-07-11 | 上海理工大学 | Method for extracting water-soluble soybean polysaccharide from low-temperature bean pulp through microwave-ultrasonic synergism |
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| CN102627700A (en) * | 2012-04-25 | 2012-08-08 | 河北农业大学 | Method for extracting polysaccharide in skirt edge and viscera of scallop through hydrolysis |
| CN104017099A (en) * | 2014-06-12 | 2014-09-03 | 苏州经贸职业技术学院 | Microwave extraction, separation and purification method of pea polysaccharide |
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| CN109749207A (en) * | 2019-02-01 | 2019-05-14 | 王玉廷 | A kind of photooxidation containing bio-based materials, biodegradable plastic and preparation method thereof |
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