CN101171956B - Method for extracting polyoses from bagasse - Google Patents
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- CN101171956B CN101171956B CN2007100316837A CN200710031683A CN101171956B CN 101171956 B CN101171956 B CN 101171956B CN 2007100316837 A CN2007100316837 A CN 2007100316837A CN 200710031683 A CN200710031683 A CN 200710031683A CN 101171956 B CN101171956 B CN 101171956B
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Abstract
The invention provides a polyhexose extraction method from the sugar cane bagasse. The method is realized by that after the degreasing processing is performed to the sugar cane bagasse, one or more of cellulolytic enzyme, papayotin and pectolytic enzyme can be hysrolyzed for 0.5 to 1.5 hours under pH value of 4 to 6 at the temperature of 40 to 80 DEG C, treated for 0.5 to 1.5 hours under the supersonic wave with the frequency of 59KHz, and filtered, and finally the polyhexose in the filtrate water is precipitated through ethanol. The method of the invention adjusts the types and the dose of the enzyme on the technology base of eumycete polyhexose extraction, and finds a low energy consumption and efficient sugar cane bagasse polyhexose extraction method under the enzyme processing and supersonic wave extraction technology.
Description
Technical field
The present invention relates to the preparation of polysaccharide compound, be specifically related to the extraction of bagasse polysaccharide.
Background technology
Bagasse is the main byproduct of sugar industry, is last major portion after the sugarcane mechanical compaction, belongs to a kind of in the agricultural solid residue, and its composition and wood materials are more or less the same, and can be used as the raw material that substitutes part timber.Provinces such as Hainan of China, Guangdong, Guangxi, Fujian, Yunnan can grow cane, and also are important product sugar provinces, and each sugar refinery all stock a large amount of bagasse, so it is significant to seek suitable way comprehensive utilization bagasse.
Contain polysaccharide in the bagasse, mainly form by five-carbon sugar and hexose.Studies show that the polysaccharide that extracts has immunostimulant, antitumor, antiviral, hypoglycemic, reducing blood-fat etc. from bagasse, have bigger development space, but its extraction process is comparatively loaded down with trivial details, use more chemical reagent, seriously polluted, energy consumption is higher.
The extracting method of existing polysaccharide has water extraction and alcohol precipitation method, microwave method, acid-base method, enzyme facture etc., and is higher to equipment requirements though newer extracting method such as microwave method has certain effect to improving extraction yield, implements to acquire a certain degree of difficulty.Though acid or alkali extraction can improve extraction yield, acid, alkali destroy the structure of polysaccharide, need through neutralization after acid, the alkali lixiviate, and program is loaded down with trivial details.The enzyme facture with respect to aforesaid method have reaction temperature and, yield height, with low cost, simple operation and other advantages, use in a large number in the extraction of polysaccharide, wait " the condition research of supersonic method and ultrasonic wave Enzymatic Extraction ganoderan " that the people delivers quietly as Zheng and disclose the method for utilizing ultrasonic wave cellulose-binding enzyme extraction ganoderan: be that 80% ethanol refluxes for 85 ℃ and took off oligose in 6 hours with 3 times of volumetric concentrations 1, the Ganoderma sporophore powder, leach solvent, filter residue is dried; 2, by 1: 20 (W: solid-liquid ratio V), 2% enzyme amount, at pH6.0,50 ℃ of following enzymolysis 20 minutes; 3,55 ℃ of supersound extraction 15 minutes; 4, with extracting solution after filtration, centrifugal, concentrated and ethanol sedimentation gets Crude polysaccharides.This method is extracted ganoderan yield height, cycle weak point, and polysaccharide content is up to 57.62% in the crude extract.But glossy ganoderma is a fungi, ganoderan is stored in the sporophore cell walls more, the main composition composition of its sporophore is Mierocrystalline cellulose, hemicellulose and xylogen, and sugarcane is a plant, and bagasse mainly is made up of holocellulose, xylogen, pentosan etc., and its fiber mainly comprises true fiber and sugarcane marrow, true fiber has more tough sclerine tissue, the then spongy structure of sugarcane marrow has bigger differently with glossy ganoderma, applies mechanically the effect that the technology of aforesaid method is difficult to obtain.
Summary of the invention
The object of the present invention is to provide a kind of method of from bagasse, extracting polysaccharide.
The present invention realizes that the technical scheme of above-mentioned purpose is:
A kind of method of from bagasse, extracting polysaccharide, this method is made up of following steps:
(1) degreasing: with the bagasse raw material with the concentration of 8～12 times of volumes more than or equal to 90% alcohol reflux 1～3 hour, filter, get filter residue and volatilize behind the solvent standby;
(2) enzyme is handled: the enzyme solution that the bagasse after the skimming treatment is soaked in 10～15 times of volumes ℃ following hydrolysis 0.5～1.5 hour in pH4～6,40～80; Described enzyme can be a kind of in cellulase, papoid, the polygalacturonase, consumption is a bagasse weight 0.5%～1.5%, also can be two or more in cellulase, papoid, the polygalacturonase, the consumption of every kind of enzyme is a bagasse weight 0.5%～1.5%, preferably cellulase and papoid, the consumption of every kind of enzyme is 1.5% of bagasse weight;
(3) supersound extraction: be to handle 0.5～1.5 hour under the ultrasonic wave of 59KHz in frequency, filter, collect filtrate;
(4) alcohol precipitation: add ethanol and make its concentration to 80～90% in filtrate, be settled out bagasse polysaccharide solid, 60～80 ℃ of vacuum-dryings.
In the aforesaid method, described enzyme treatment step is a enzyme solution that the bagasse after the skimming treatment is soaked in 10～15 times of volumes pH5.5,60 ℃ of following hydrolysis 60 minutes.
The principle of the inventive method is: utilize enzyme to handle bagasse, the reaction conditions gentleness, can not destroy the bagasse polysaccharide structures, utilize cavitation effect of ultrasonic waves to quicken the stripping of polysaccharide then, hyperacoustic in addition second-order effect such as mechanical vibration, emulsification, spread, smash, diffusion that chemical effect etc. also can be quickened polysaccharide discharges and fully and solvent, help extracting; Ultrasonic-assisted extraction has the extraction time weak point, and solvent load is few, and the extraction yield height helps further making with extra care advantages such as purification, and need not heating, is suitable for extracting heat-sensitive materials.
Though with enzyme processing and ultrasonic extraction fungus polysaccharide has been this area means commonly used, because bagasse component and structure and fungi have bigger difference, adopt the technology identical to extract the bagasse polysaccharide with extracting fungus polysaccharide, effect is obviously not good enough.The present invention has selected the enzyme that the bagasse component is had better Degradation for use, and the collocation and the consumption of various enzymes have been optimized, make Mierocrystalline cellulose, xylogen and range protein in its bagasse of fully degrading, also adjusted the condition of ultrasonic extraction simultaneously, quicken the stripping of polysaccharide, not only the extraction yield of bagasse polysaccharide improves 50～100% than traditional method, and polysaccharide content is higher in the extract, and active polysaccharide is retained.
Embodiment
Further specify effect of the present invention below in conjunction with embodiment.
Embodiment 1
With bagasse meal 1Kg, add 8 liters of straight alcohols, refluxing extraction 1 hour is filtered and is collected filter residue.Add 10 times of water, add cellulase 15 grams, adjust pH to 5.5 is with the filter residue mixing, 60 ℃ are incubated 60 minutes, supersound process 60 minutes is filtered, and filtrate is polysaccharide extraction liquid, adding ethanol adjusting determining alcohol after extracting solution concentrates is 90%, placement is spent the night, and will precipitate 60 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 85g.
Embodiment 2
With bagasse meal 1Kg, add 10 liter of 90% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add cellulase 5 grams, adjust pH to 4.0 is with the filter residue mixing, 80 ℃ are incubated 30 minutes, supersound process 90 minutes is filtered, and filtrate is polysaccharide extraction liquid, adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, placement is spent the night, and will precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 65g.
Embodiment 3
With bagasse meal 1Kg, add 10 liter of 90% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add cellulase 10 grams, adjust pH to 6.0 is with the filter residue mixing, 40 ℃ are incubated 90 minutes, supersound process 30 minutes is filtered, and filtrate is polysaccharide extraction liquid, adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, placement is spent the night, and will precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 64g.
Embodiment 4
With bagasse meal 1Kg, add 10 liters of ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add polygalacturonase 10 grams, adjust pH to 4.5 is with the filter residue mixing, 60 ℃ are incubated 60 minutes, supersound process 60 minutes is filtered, and filtrate is polysaccharide extraction liquid, adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, placement is spent the night, and will precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 72g.
Embodiment 5
With bagasse meal 1Kg, add 10 liter of 95% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add polygalacturonase 5 grams, adjust pH to 4.0 is with the filter residue mixing, 40 ℃ are incubated 80 minutes, supersound process 30 minutes is filtered, and filtrate is polysaccharide extraction liquid, adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, placement is spent the night, and will precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 70g.
Embodiment 6
With bagasse meal 1Kg, add 10 liter of 95% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add polygalacturonase 1.5 grams, adjust pH to 6.0 is with the filter residue mixing, 50 ℃ are incubated 40 minutes, supersound process 90 minutes is filtered, and filtrate is polysaccharide extraction liquid, adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, placement is spent the night, and will precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 68g.
Embodiment 7
With bagasse meal 1Kg, add 12 liter of 90% ethanol, refluxing extraction 3 hours is filtered and is collected filter residue.Add 15 times of water, add papoid 10 grams, adjust pH to 4.5 is with the filter residue mixing, 60 ℃ are incubated 60 minutes, supersound process 60 minutes is filtered, and filtrate is polysaccharide extraction liquid, adding ethanol adjusting determining alcohol after extracting solution concentrates is 90%, placement is spent the night, and will precipitate 80 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 82g.
Embodiment 8
With bagasse meal 1Kg, add 10 liter of 95% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add papoid 5 grams, adjust pH to 4.0 is with the filter residue mixing, 40 ℃ are incubated 80 minutes, supersound process 30 minutes is filtered, and filtrate is polysaccharide extraction liquid, adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, placement is spent the night, and will precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 68g.
Embodiment 9
With bagasse meal 1Kg, add 10 liter of 90% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add papoid 1.5 grams, adjust pH to 6.0 is with the filter residue mixing, 50 ℃ are incubated 40 minutes, supersound process 90 minutes is filtered, and filtrate is polysaccharide extraction liquid, adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, placement is spent the night, and will precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 73g.
Embodiment 10
With bagasse meal 1Kg, add 10 liter of 90% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add cellulase 15 grams, polygalacturonase 10 grams, adjust pH to 5.5, with the filter residue mixing, 60 ℃ are incubated 60 minutes, supersound process 60 minutes, filter, filtrate is polysaccharide extraction liquid, and adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, and placement is spent the night, to precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 86g.
Embodiment 11
With bagasse meal 1Kg, add 10 liter of 90% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add cellulase 15 grams, polygalacturonase 15 grams, adjust pH to 4.0, with the filter residue mixing, 60 ℃ are incubated 60 minutes, supersound process 90 minutes, filter, filtrate is polysaccharide extraction liquid, and adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, and placement is spent the night, to precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 89g.
Embodiment 12
With bagasse meal 1Kg, add 10 liter of 90% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add cellulase 10 grams, polygalacturonase 15 grams, adjust pH to 6.0, with the filter residue mixing, 60 ℃ are incubated 60 minutes, supersound process 30 minutes, filter, filtrate is polysaccharide extraction liquid, and adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, and placement is spent the night, to precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 97g.
Embodiment 13
With bagasse meal 1Kg, add 10 liter of 90% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add papoid 15 grams, polygalacturonase 15 grams, adjust pH to 5.5, with the filter residue mixing, 60 ℃ are incubated 60 minutes, supersound process 60 minutes, filter, filtrate is polysaccharide extraction liquid, and adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, and placement is spent the night, to precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 79g.
Embodiment 14
With bagasse meal 1Kg, add 10 liter of 90% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add papoid 15 grams, polygalacturonase 10 grams, adjust pH to 4.0, with the filter residue mixing, 80 ℃ are incubated 30 minutes, supersound process 90 minutes, filter, filtrate is polysaccharide extraction liquid, and adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, and placement is spent the night, to precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 81g.
Embodiment 15
With bagasse meal 1Kg, add 10 liter of 90% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add papoid 10 grams, polygalacturonase 15 grams, adjust pH to 6.0, with the filter residue mixing, 40 ℃ are incubated 90 minutes, supersound process 30 minutes, filter, filtrate is polysaccharide extraction liquid, and adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, and placement is spent the night, to precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 80g.
Embodiment 16
With bagasse meal 1Kg, add 10 liter of 90% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add papoid 15 grams, cellulase 15 grams, adjust pH to 5.5, with the filter residue mixing, 60 ℃ are incubated 60 minutes, supersound process 60 minutes, filter, filtrate is polysaccharide extraction liquid, and adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, and placement is spent the night, to precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 113g.
Embodiment 17
With bagasse meal 1Kg, add 10 liter of 90% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add papoid 15 grams, cellulase 10 grams, adjust pH to 4.0, with the filter residue mixing, 80 ℃ are incubated 30 minutes, supersound process 90 minutes, filter, filtrate is polysaccharide extraction liquid, and adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, and placement is spent the night, to precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 99g.
Embodiment 18
With bagasse meal 1Kg, add 10 liter of 90% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add papoid 10 grams, cellulase 15 grams, adjust pH to 6.0, with the filter residue mixing, 40 ℃ are incubated 90 minutes, supersound process 30 minutes, filter, filtrate is polysaccharide extraction liquid, and adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, and placement is spent the night, to precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 98g.
Embodiment 19
With bagasse meal 1Kg, add 10 liter of 90% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add papoid 15 grams, cellulase 15 grams, polygalacturonase 15 grams, adjust pH to 5.5 is with the filter residue mixing, 60 ℃ are incubated 60 minutes, supersound process 60 minutes is filtered, and filtrate is polysaccharide extraction liquid, adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, placement is spent the night, and will precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 98g.
Embodiment 20
With bagasse meal 1Kg, add 10 liter of 90% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add papoid 15 grams, cellulase 10 grams, polygalacturonase 10 grams, adjust pH to 4.0 is with the filter residue mixing, 80 ℃ are incubated 30 minutes, supersound process 90 minutes is filtered, and filtrate is polysaccharide extraction liquid, adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, placement is spent the night, and will precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 107g.
Embodiment 21
With bagasse meal 1Kg, add 10 liter of 90% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, add papoid 10 grams, cellulase 15 grams, polygalacturonase 15 grams, adjust pH to 6.0 is with the filter residue mixing, 40 ℃ are incubated 90 minutes, supersound process 30 minutes is filtered, and filtrate is polysaccharide extraction liquid, adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, placement is spent the night, and will precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 104g.
Embodiment 22 (comparative example)
With bagasse meal 1Kg, add 10 liter of 90% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, adjust pH to 6.0, with the filter residue mixing, 40 ℃ of insulations 90 minutes are filtered, filtrate is polysaccharide extraction liquid, adding ethanol after extracting solution concentrates, to regulate determining alcohol be 85%, placement is spent the night, and will precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 43g.
Embodiment 23 (comparative example)
With bagasse meal 1Kg, add 10 liter of 90% ethanol, refluxing extraction 2 hours is filtered and is collected filter residue.Add 12 times of water, adjust pH to 6.0, with the filter residue mixing, 40 ℃ are incubated 90 minutes, supersound process 30 minutes is filtered, and filtrate is polysaccharide extraction liquid, and adding ethanol adjusting determining alcohol after extracting solution concentrates is 85%, placement is spent the night, and will precipitate 70 ℃ of vacuum-dryings, pulverize bagasse polysaccharide crude 58g.
Claims (4)
1. method of from bagasse, extracting polysaccharide, this method is made up of following steps:
(1) degreasing: with the bagasse raw material with the concentration of 8～12 times of volumes more than or equal to 90% alcohol reflux 1～3 hour, filter, get filter residue and volatilize behind the solvent standby;
(2) enzyme is handled: the enzyme solution that the bagasse after the skimming treatment is soaked in 10～15 times of volumes ℃ following hydrolysis 0.5～1.5 hour in pH4～6,40～80; Described enzyme is one or more in cellulase, papoid, the polygalacturonase, and the consumption of every kind of enzyme is a bagasse weight 0.5%～1.5%;
(3) supersound extraction: be to handle 0.5～1.5 hour under the ultrasonic wave of 59KHz in frequency, filter, collect filtrate;
(4) alcohol precipitation: add ethanol and make its concentration to 80～90% in filtrate, be settled out bagasse polysaccharide solid, 60～80 ℃ of vacuum-dryings.
2. method according to claim 1 is characterized in that enzyme is cellulase and papoid, and the consumption of every kind of enzyme is 1.5% of bagasse weight.
3. method according to claim 1 is characterized in that described enzyme treatment step is a enzyme solution that the bagasse after the skimming treatment is soaked in 10～15 times of volumes pH5.5,60 ℃ of following hydrolysis 60 minutes.
4. method according to claim 1, the time that it is characterized in that described supersound extraction is 60 minutes.
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| CN107529517A (en) * | 2016-07-09 | 2018-01-02 | 王玲燕 | A kind of method that nitrogen carbon molecular sieve is prepared by bagasse |
| CN108359696A (en) * | 2018-02-28 | 2018-08-03 | 苏州昆蓝生物科技有限公司 | A kind of preparation method of xylo-oligosaccharide |
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