CN103525953B - Method for preparing fructo-oligose through acidolysis - Google Patents
Method for preparing fructo-oligose through acidolysis Download PDFInfo
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Abstract
The invention relates to a preparation method of high-purity fructo-oligose, particularly to a method for preparing fructo-oligose through acidolysis of synanthrin. The method comprises the steps of adding water with certain proportion into pretreated jerusalem artichoke, pulping, adding concentrated sulfuric acid with concentration of 98% into jerusalem artichoke pulp to regulate pH value to be 1-4, carrying out acidolysis for 1-3h at 60-130 DEG C, and performing rough filtration, nanofiltration, ultrafiltration, decoloring, desalting and drying to acid-hydrolyzed liquid to obtain high-purity fructo-oligose powder. The method has the characteristics that sulfuric acid is used for acidolysis of synanthrin to produce fructo-oligose and the enzyme technology is not adopted, so that the production cost is lowered; the nanofiltration and ultrafiltration separation technologies are adopted to separate fructo-oligose, so that large-scale industrial production is realized; the purity of fructo-oligose can reach more than 98%.
Description
Technical field
The present invention relates to the preparation method of high-purity fructo oligosaccharides, particularly relate to a kind of method that oligofructose is prepared in acidolysis.
Background technology
Oligofructose (Fructiooligosaccharides, be called for short FOS) be the linear oligosacchardides become by fructosyl glucosyl group, its structure has two kinds of forms: a kind of be sucrose molecules residue of fructose on by β (2-1) glycosidic link connect 1-8 molecule fructosyl form, its structural formula is expressed as GF
2-GF
9(G is glucosyl group, and F is fructosyl); Another kind is formed by connecting by β (2-1) glycosidic link by 3-9 residue of fructose, and its structural formula is expressed as F
3-F
9.Oligofructose is a kind of natural active matter, has regulating intestinal canal flora, propagation bifidus bacillus, promote the absorption of calcium, adjusting blood lipid, immunomodulatory, the novel sweetener of the nourishing functions such as anti-dental caries, is described as the additive of new generation of most potentiality after the microbiotic epoch---growth-promoting material; Oligofructose or a kind of water miscible food fibre, can reduce serum cholesterol and content of triglyceride, takes in oligofructose and glucose level can not be caused to fluctuate, can be used as the sweeting agent of hypertension, diabetes and obesity patient.
At present, the production method of oligofructose mainly contains two kinds: 1. sucrose inversion method, this method in nineteen eighty-two at Japanese industry, with the sucrose solution of ferment treatment high density, obtain the solution of oligofructose contents on dry basis 55%, all the other 45% be fructose, glucose sugar and sucrose, obtain through separation and purification the oligofructose that purity is 95%.This method due to separating-purifying difficulty large, Chinese Enterprise can only produce the oligofructose product of 55% substantially.2. synanthrin hydrolysis method, this method is adopted in a large number by Europe at present.This method extracts synanthrin from witloof, be hydrolyzed through synanthrin restriction endonuclease, obtain the mixture of oligofructose, glucose, sucrose, oligofructose is obtained through separating-purifying, but because in enzymolysis product, the contents on dry basis of oligofructose also only has 55%, monose and sucrose content are too high, separation difficulty, can't produce the product that oligofructose content is greater than 95%.
There is same deficiency in above two kinds of technology, namely producing enzyme used only has few unit to produce, and as the then more difficult preparation of pure enzyme, use enzyme-squash techniqued oligofructose, cost is high, enzymolysis product be difficult to control, monose and sucrose content high, separating-purifying difficulty is large.
Summary of the invention
The object of this invention is to provide a kind of cost low, simple to operate, the method for oligofructose is prepared in a kind of acidolysis being suitable for industrialization production.
For achieving the above object, the present invention adopts following technical scheme to be:
A kind of preparation method of high-purity fructo oligosaccharides: pretreated jerusalem artichoke is pulled an oar than the solid-liquid ratio for 1:1-1:2 according to jerusalem artichoke and quality, then in jerusalem artichoke slurry, add concentration is that 98% vitriol oil adjusts pH to be 1-4, acidolysis 1-3h under 60-130 DEG C of condition, acid hydrolysis solution obtains high-purity fructo oligosaccharides powder again after coarse filtration, nanofiltration, ultrafiltration, decolouring, desalination, drying.
Pre-treatment is by jerusalem artichoke cleaning, peeling, chopping process.
Described making beating refers to and breaks into pulpous state by putting in food processor than the solid-liquid ratio for 1:1-1:2 according to jerusalem artichoke and quality, is jerusalem artichoke slurry.
The sulfuric acid concentration that described acidolysis adopts is 98%; Add-on for 1-4 is suitable, is the suitableeest with mixed solution final pH when especially equaling 2 with pH.
By described after sulfuric acid solution jerusalem artichoke acid hydrolysis solution flame filter press cross and filter jerusalem artichoke slag, collect filtrate; Be the nanofiltration membrane room temperature filtration of 200-300 by the filtrate molecular weight cut-off of collection, collect concentrated solution; The concentrated solution of collection is filtered by the ultra-filtration membrane room temperature that molecular weight cut-off is 1500 again, collects permeate; The permeate of collecting is through negatively charged ion macroporous adsorbent resin at room temperature with the flow velocity wash-out of 0.5-2.5ml/min, and moving phase is water, collects elutriant; By the elutriant of negatively charged ion macroporous adsorbent resin wash-out desolventing technology successively through strong cat ion exchange column and strong anion exchange column wash-out, elution flow rate is 0.5-2.5ml/min, and moving phase is water, obtains elutriant; The drying of elutriant spray-drier obtains the oligofructose that purity is greater than 98%.
Described negatively charged ion macroporous adsorbent resin type, strong cat ion exchange column, strong anion exchange column model are followed successively by D301, D072, D201.
Further, after jerusalem artichoke cleaning, peeling, chopping, pull an oar than the solid-liquid ratio input food handler for 1:1.2 according to jerusalem artichoke and quality, add in jerusalem artichoke slurry concentration be 98% the vitriol oil be 2 to pH, be placed in acidolysis 60min under 100 DEG C of conditions, acid hydrolysis solution flame filter press is crossed and is filtered jerusalem artichoke slag, collects filtrate; Be the nanofiltration membrane room temperature filtration of 200-300 by the filtrate molecular weight cut-off of collection, collect concentrated solution; The concentrated solution of collection is filtered by the ultra-filtration membrane room temperature that molecular weight cut-off is 1500 again, collects permeate; The permeate of collecting at room temperature is decoloured with the flow velocity wash-out of 2.0ml/min through negatively charged ion macroporous adsorbent resin, and moving phase is water, collects elutriant; By the elutriant of negatively charged ion macroporous adsorbent resin wash-out desolventing technology successively through strong cat ion exchange column and strong anion exchange column wash-out desalination, elution flow rate is 2.0ml/min, and moving phase is water, obtains elutriant; Elutriant is dry with spray-drier, and inlet temperature is 120 DEG C, finally obtains the oligofructose that purity is 99%.
The advantage that the present invention has:
1., owing to lacking the restriction endonuclease of degraded synanthrin that is efficiently single-minded, that be suitable for suitability for industrialized production at present, the present invention uses sulfuric acid solution synanthrin cheap and easy to get to produce oligofructose.Therefore, the present invention's acid hydrolyzation reduces production cost, makes the suitability for industrialized production of oligofructose become possibility;
2. the present invention's acid hydrolyzation, although introduce sulfate ion in process, can remove through strong anion exchange column, and strong anion exchange column uses at every turn and can repeatedly use after simple process, and coefficient of losses is low;
3. the processing condition set by the present invention, can make by product hydroxymethyl furfural content < 1.5%;
4. the present invention uses nanofiltration membrane separation method separating oligomeric fructose, and step is simple, easy to operate, and process is easy to control, and facilitates large-scale industrial to produce;
5. the oligofructose purity adopting the present invention to obtain is high, can reach more than 98%.
Embodiment:
Embodiment 1
With fresh jerusalem artichoke for raw material, specifically press step and carry out:
1., after choosing fresh jerusalem artichoke 500g cleaning, peeling, chopping, pull an oar with input food handler while of 600g water;
2. in jerusalem artichoke slurry, to add the vitriol oil to pH be 2, is placed in acidolysis 60min under 100 DEG C of conditions;
3. jerusalem artichoke acid hydrolysis solution flame filter press is crossed and is filtered jerusalem artichoke slag, collects filtrate;
4. be the nanofiltration membrane room temperature filtration of 200-300 by the filtrate molecular weight cut-off of collection, collect concentrated solution;
5. the concentrated solution of collection is filtered by the ultra-filtration membrane room temperature that molecular weight cut-off is 1500 again, collect permeate;
6. the permeate of collecting at room temperature is decoloured with the flow velocity wash-out of 2.0ml/min through negatively charged ion macroporous adsorbent resin, and moving phase is water, collects elutriant;
7. by the elutriant of negatively charged ion macroporous adsorbent resin wash-out desolventing technology successively through strong cat ion exchange column and strong anion exchange column wash-out desalination, elution flow rate is 2.0ml/min, and moving phase is water, obtains elutriant;
8. elutriant is dry with spray-drier, and inlet temperature is 120 DEG C, finally obtains the oligofructose that purity is 99%.
The oligofructose obtained by aforesaid method, effect is as table 1.Simultaneously through ultrafiltration membrance filter gained to the polymer synanthrin except oligofructose except can be used as fat material, in food interpolation, also have good application prospect.
Embodiment 2:
With fresh jerusalem artichoke for raw material, specifically press step and carry out:
1., after choosing fresh jerusalem artichoke 50kg cleaning, peeling, chopping, pull an oar with input food handler while of 100kg water;
2. in jerusalem artichoke slurry, to add the vitriol oil to pH be 2, is placed in acidolysis 150min under 60 DEG C of conditions;
3. jerusalem artichoke acid hydrolysis solution flame filter press is crossed and is filtered jerusalem artichoke slag, collects filtrate;
4. be the nanofiltration membrane room temperature filtration of 200-300 by the filtrate molecular weight cut-off of collection, collect concentrated solution;
5. the concentrated solution of collection is filtered by the ultra-filtration membrane room temperature that molecular weight cut-off is 1500 again, collect permeate;
6. the permeate of collecting at room temperature is decoloured with the flow velocity wash-out of 2.5ml/min through negatively charged ion macroporous adsorbent resin, and moving phase is water, collects elutriant;
7. by the elutriant of negatively charged ion macroporous adsorbent resin wash-out desolventing technology successively through strong cat ion exchange column and strong anion exchange column wash-out desalination, elution flow rate is 2.5ml/min, and moving phase is water, obtains elutriant;
8. elutriant is dry with spray-drier, and inlet temperature is 130 DEG C, finally obtains the oligofructose that purity is 98%.
The oligofructose obtained by aforesaid method, effect is as table 1.
Embodiment 3:
With fresh jerusalem artichoke for raw material, specifically press step and carry out:
1., after choosing fresh jerusalem artichoke 50kg cleaning, peeling, chopping, pull an oar with input food handler while of 50kg water;
2. in jerusalem artichoke slurry, to add the vitriol oil to pH be 3, is placed in acidolysis 100min under 100 DEG C of conditions;
3. jerusalem artichoke acid hydrolysis solution flame filter press is crossed and is filtered jerusalem artichoke slag, collects filtrate;
4. be the nanofiltration membrane room temperature filtration of 200-300 by the filtrate molecular weight cut-off of collection, collect concentrated solution;
5. the concentrated solution of collection is filtered by the ultra-filtration membrane room temperature that molecular weight cut-off is 1500 again, collect permeate;
6. the permeate of collecting at room temperature is decoloured with the flow velocity wash-out of 1.5ml/min through negatively charged ion macroporous adsorbent resin, and moving phase is water, collects elutriant;
7. by the elutriant of negatively charged ion macroporous adsorbent resin wash-out desolventing technology successively through strong cat ion exchange column and strong anion exchange column wash-out desalination, elution flow rate is 1.5ml/min, and moving phase is water, obtains elutriant;
8. elutriant is dry with spray-drier, and inlet temperature is 140 DEG C, finally obtains the oligofructose that purity is 98%.
The oligofructose obtained by aforesaid method, effect is as table 1.
Embodiment 4:
With fresh jerusalem artichoke for raw material, specifically press step and carry out:
1., after fresh jerusalem artichoke 80kg cleaning, peeling, chopping, pull an oar with input food handler while of 100kg water;
2. in jerusalem artichoke slurry, to add the vitriol oil to pH be 3.5, is placed in acidolysis 100min under 100 DEG C of conditions;
3. jerusalem artichoke acid hydrolysis solution flame filter press is crossed and is filtered jerusalem artichoke slag, collects filtrate;
4. be the nanofiltration membrane room temperature filtration of 200-300 by the filtrate molecular weight cut-off of collection, collect concentrated solution;
5. the concentrated solution of collection is filtered by the ultra-filtration membrane room temperature that molecular weight cut-off is 1500 again, collect permeate;
6. the permeate of collecting at room temperature is decoloured with the flow velocity wash-out of 1.2ml/min through negatively charged ion macroporous adsorbent resin, and moving phase is water, collects elutriant;
7. by the elutriant of negatively charged ion macroporous adsorbent resin wash-out desolventing technology successively through strong cat ion exchange column and strong anion exchange column wash-out desalination, elution flow rate is 1.2ml/min, and moving phase is water, obtains elutriant;
8. elutriant is dry with spray-drier, and inlet temperature is 120 DEG C, finally obtains the oligofructose that purity is 98%.
The oligofructose obtained by aforesaid method, effect is as table 1.
Table 1: each embodiment effect
Claims (5)
1. the preparation method of a high-purity fructo oligosaccharides, it is characterized in that: pretreated jerusalem artichoke is pulled an oar than the solid-liquid ratio for 1:1-1:2 according to jerusalem artichoke and quality, then in jerusalem artichoke slurry, adding 98% vitriol oil adjusts pH to be 1-4, acidolysis 1-3h under 60-130 DEG C of condition, acid hydrolysis solution obtains high-purity fructo oligosaccharides powder again after coarse filtration, nanofiltration, ultrafiltration, decolouring, desalination, drying;
Described pre-treatment is by jerusalem artichoke cleaning, peeling, chopping process.
2. by the preparation method of high-purity fructo oligosaccharides according to claim 1, it is characterized in that: described making beating refers to and breaks into pulpous state by putting in food processor than the solid-liquid ratio for 1:1-1:2 according to jerusalem artichoke and quality, is jerusalem artichoke slurry.
3., by the preparation method of high-purity fructo oligosaccharides according to claim 1, it is characterized in that: by described after sulfuric acid solution jerusalem artichoke acid hydrolysis solution flame filter press cross and filter jerusalem artichoke slag, collect filtrate; Be the nanofiltration membrane room temperature filtration of 200-300 by the filtrate molecular weight cut-off of collection, collect concentrated solution; Be the ultra-filtration membrane room temperature filtration of 1500 by the concentrated solution molecular weight cut-off of collection, collect permeate; The permeate of collecting at room temperature is decoloured with the flow velocity wash-out of 0.5-2.5ml/min through negatively charged ion macroporous adsorbent resin, and moving phase is water, collects elutriant; By the elutriant of negatively charged ion macroporous adsorbent resin wash-out desolventing technology successively through strong cat ion exchange column and strong anion exchange column wash-out desalination, elution flow rate is 0.5-2.5ml/min, and moving phase is water, obtains elutriant; Elutriant is dry with spray-drier, and inlet temperature is 100-150 DEG C.
4., by the preparation method of high-purity fructo oligosaccharides according to claim 3, it is characterized in that: described negatively charged ion macroporous adsorbent resin, strong cat ion exchange column, strong anion exchange column model are followed successively by D301, D072, D201.
5. by the preparation method of high-purity fructo oligosaccharides according to claim 1, it is characterized in that: after jerusalem artichoke cleaning, peeling, chopping, pull an oar than the solid-liquid ratio input food handler for 1:1.2 according to jerusalem artichoke and quality, then in jerusalem artichoke slurry in add concentration be 98% the vitriol oil adjust pH be 2, be placed in acidolysis 60min under 100 DEG C of conditions, acid hydrolysis solution flame filter press is crossed and is filtered jerusalem artichoke slag, collects filtrate; Be the nanofiltration membrane room temperature filtration of 200-300 by the filtrate molecular weight cut-off of collection, collect concentrated solution; The concentrated solution of collection is filtered by the ultra-filtration membrane room temperature that molecular weight cut-off is 1500 again, collects permeate; The permeate of collecting at room temperature is decoloured with the flow velocity wash-out of 2.0ml/min through negatively charged ion macroporous adsorbent resin, and moving phase is water, collects elutriant; By the elutriant of negatively charged ion macroporous adsorbent resin wash-out desolventing technology successively through strong cat ion exchange column and strong anion exchange column wash-out desalination, elution flow rate is 2.0ml/min, and moving phase is water, obtains elutriant; Elutriant is dry with spray-drier, and inlet temperature is 120 DEG C, finally obtains the oligofructose that purity is 99%.
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| CN104531809A (en) * | 2014-12-04 | 2015-04-22 | 青海威德生物技术有限公司 | Preparation and purification method of fructo-oligosaccharide |
| CN105106043B (en) * | 2015-07-16 | 2017-10-20 | 山东省分析测试中心 | Fragrant mouthwash of a kind of peony anti-inflammatory deodorization and preparation method thereof |
| CN105418695B (en) * | 2015-12-30 | 2019-02-15 | 重庆骄王天然产物股份有限公司 | A kind of method of UF membrane production liquid oligomeric fructose |
| CN105861594B (en) * | 2016-05-23 | 2020-04-14 | 上海艾苛密进出口有限公司 | Preparation method of fructo-oligosaccharide |
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| CN102093437B (en) * | 2010-12-20 | 2014-03-19 | 大兴安岭林格贝有机食品有限责任公司 | Method for enriching and purifying fructooligosaccharide in witloof |
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