CN103981236A - Preparation method of non-synthesized fructooligosaccharide - Google Patents
Preparation method of non-synthesized fructooligosaccharide Download PDFInfo
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- CN103981236A CN103981236A CN201410217925.1A CN201410217925A CN103981236A CN 103981236 A CN103981236 A CN 103981236A CN 201410217925 A CN201410217925 A CN 201410217925A CN 103981236 A CN103981236 A CN 103981236A
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Abstract
The invention discloses a preparation method of non-synthesized fructooligosaccharide. The preparation method comprises the following steps of (1) carrying out enzymolysis on an inulin solution, and filtering an enzymolysis product to obtain a filtrate; (2) decolorizing the filtrate; (3) flocculating the decolorized filtrate; (4) after flocculating and filtering, desalting by using ion exchange resin, removing impurities, eliminating odor and purifying; (5) evaporating, concentrating and spray-drying the product to obtain fructooligosaccharide. The preparation method of the non-synthesized fructooligosaccharide is used for preparing 95-97% of fructooligosaccharide with the fructose polymerization degree of 2-9 by utilizing the partial hydrolysis action of an incision enzyme of inulin; in addition, compared with a sucrose conversion method, the preparation method has the advantages of simple process, few byproducts, high conversion rate and the like.
Description
Technical field
The preparation method who the present invention relates to a kind of oligofructose, belongs to food processing field, is specifically related to a kind of preparation method of non-synthesis of oligonucleotides fructose.
Background technology
Oligofructose is a kind of functional oligose, and its sugariness can reach 0.6 times of sucrose, has both kept the pure fragrant and sweet taste of sucrose, salubriouser than sucrose again, and has the adipose fragrance of class and tasty and refreshing soapy feeling.Oligofructose is a kind of water-soluble dietary fibre, in large intestine, by fermentation using bacteria, is generated Pfansteihl, can solubilize calcium, the mineral substance such as iron, zinc, promote the absorption of human body to mineral substance; To there is regulating intestinal canal flora, propagation bifidus bacillus, regulate blood fat, improve immunizing power, the novel sweetener of the nourishing functions such as anti-dental caries, has been applied to many production fields such as milk-product, lactobacillus drink, solid beverage, candy, biscuit, bread, jelly, cold drink, healthcare products.
At present, the industrialized preparing process of oligofructose mainly be take sucrose as raw material manufacture, under concentration 50%～60%, pH5.5,60 ℃ of conditions, through the effect of the fructosyl transferase of microorganism, be transformed, the shortcoming of this method is: its byproduct of reaction-glucose-and be the inhibitor of enzyme, reaction is carried out not thorough, in mixed platform thing, contain a large amount of dextrose plus saccharoses, low conversion rate, oligofructose only accounts for 55%～60% of total amount, end product needs refining and edulcoration, and complex process, production cost are high.
Therefore, how the preparation technology of oligofructose is improved, become people's problem demanding prompt solution.
Summary of the invention
Given this, the object of the present invention is to provide a kind of preparation method of non-synthesis of oligonucleotides fructose, at least to solve, prepare the problems such as the low conversion rate that exists in oligofructose method, complex process, production cost height in the past.
Technical scheme provided by the invention is: a kind of preparation method of non-synthesis of oligonucleotides fructose, it is characterized in that, and by following steps, be prepared from:
1) inulin solution is carried out to enzymolysis, enzymolysis product is filtered, obtain filtrate;
2) filtrate is decoloured processing;
3) filtrate after decolouring processing is carried out to flocculation treatment;
4), after flocculation filtration, spent ion exchange resin desalination, carries out removal of impurities, de-taste purifying;
5) above-mentioned product is carried out to evaporation concentration, spraying is dry, makes oligofructose.
Preferably, in described step 1), the concentration of inulin solution is 40 ~ 60wt%.
Further preferably, the enzyme in described step 1) is endoinulase, and its source can be microorganism or plant.Endoinulase cuts off glycosidic link at random from inulin intramolecule, and the primary product of hydrolysis is the oligofructose of the polymerization degree 2～9, and the temperature of enzyme digestion reaction is 50～65 ℃, and the reaction times is 18 ~ 22h.
Further preferably, the temperature of described enzyme digestion reaction is 55～59 ℃, and the reaction times is 20h.
Further preferably, described step 2) in, decolouring is processed and is specially: in filtrate, add gac, and the addition of the gac 0.1～5wt% that is reaction-ure mixture.
Further preferably, describedly by adding the gac processing of decolour, be specially: in temperature, be to be incubated 2～65min under 40～90 ℃ of conditions.
Further preferably, in described step 3), flocculation treatment is specially: add the PAM flocculation agent of reaction-ure mixture 0.05～0.2wt%, under whipped state, at 45～75 ℃, react 2～65min; After filtration, make flocks and the liquid separation of generation.The floc size that PAM produces is larger, is more conducive to improve the speed of sedimentation and filtration.
Further preferably, in described step 4), desalting treatment is specially: described step 4) intermediate ion exchange resin desalting treatment is specially: allow material by four resin filter beds of sun-male-female-the moon, carry out desalination successively, and controlling its flow velocity is 1～5BV/h, and initial charge temperature is 40～75 ℃.
Further preferably, in described step 5), process and be specially: in described step 5), the dry detailed process of evaporation concentration and spraying is: evaporation concentration is to react 30～90min in 60～90 ℃ of evaporating pots, keep during this time vacuum tightness more than 500 mmhg, be less than 18% to material moisture; Carry out subsequently spray drying treatment, inlet temperature is controlled at 120～160 ℃, is dried to moisture and is less than 5%.
The preparation method of non-synthesis of oligonucleotides fructose provided by the invention, utilize the partial hydrolysis effect of endo-inulinase to generate the oligofructose that the fructose polymerization degree is 2～9, content can be up to 95%～97%, with sucrose inversion method, compare, the present invention has that technique is simple, by product is few, transformation efficiency advantages of higher.
Embodiment
With specific embodiments, the present invention is further explained below, but is not limited to the present invention.
In order to solve the problems such as the low conversion rate that exists in the preparation method of oligofructose in the past, complex process, production cost height, the invention provides a kind of preparation method of non-synthesis of oligonucleotides fructose, specifically by following steps, be prepared from:
1) inulin solution is hydrolyzed through endoinulase, enzymolysis product is filtered, obtain filtrate;
2) by filtrate with the gac processing of decolouring;
3) after decolouring, with PAM flocculation agent, carry out flocculation treatment;
4) by ion exchange resin, carry out desalination, further removal of impurities, de-taste, purifying oligofructose;
5) above-mentioned product is carried out to evaporation concentration, spraying is dry, makes oligofructose.
The method of preparing non-synthesis of oligonucleotides fructose in the present invention, take inulin as raw material, utilize endoinulase method to produce oligofructose, wherein, in step 1), inulin solution is carried out to enzymolysis, endoinulase cuts off glycosidic link at random from inulin intramolecule, the oligofructose that the generation polymerization degree is 2～9, through ultrafiltration membrance filter, a small amount of glucose and fructose are filtered out, leave the effective constituent polymerization degree and be 2～9 oligofructose; Step 2) in, utilize the adsorption of gac, get rid of most of coloring matter; In step 3), with PAM, carry out flocculation treatment, by the charged group on its macromolecular chain, with adsorption bridging and charge neutrality mode, with protein pectin etc., intermolecular interaction occurs, by thick ion aggregation in solution together, thereby realize rapid subsidence; In step 4), spent ion exchange resin carries out desalination, further removal of impurities, de-taste, purifying oligofructose; Step 5) is first carried out evaporation concentration by reaction product, removes most of moisture wherein, then it is dry to spray, and finally makes high-purity fructo oligosaccharides.
In order to improve the effect of enzymolysis in step 1), the concentration of inulin solution is 40～60wt%, and the katalaze enzyme in described enzymolysis process is endoinulase.Compared to the non-reduced end from inulin molecule of exoinulinase, cut in turn fructose molecule and it is hydrolyzed into fructose and glucose the most at last, the mechanism of action of endoinulase is to cut off at random glycosidic link from inulin intramolecule, and product is mainly the oligofructose of the polymerization degree 2～9.
In order to remove the pigment after inulin enzymolysis, step 2) having carried out decolouring processes, prevent from decolouring in treating processes and introduce other foreign material in filtered liquid, preferred physical decolorization method, in filtrate, add gac, the adsorptive power of the super large specific surface area by gac, is adsorbed onto the pigment in filtrate in gac, realizes the object of decolouring.
In order to reach the best effect of spent ion exchange resin desalination in step 4), before, added the link of use PAM flocculation agent in step 3), wherein, PAM flocculation agent chemical name polyacrylamide, for high molecular weight water soluble polymer, be insoluble to most of organic solvents, there is good flocculence, can reduce the frictional resistance between liquid, commercially available.Charged group on PAM macromolecular chain is with adsorption bridging and charge neutrality mode, with protein pectin etc., intermolecular interaction occurs, and by thick ion aggregation in solution together, thereby realizes rapid subsidence;
Ion exchange resin in step 4) is macroreticular ion exchange resin, by this link, carries out desalting treatment, further removal of impurities, de-taste, purifying oligofructose.Material is successively by four resin filter beds of sun-male-female-the moon, and controlling its flow velocity is 1～5BV/h, and initial charge temperature is 40～75 ℃.
In step 5), evaporation concentration and the dry preferred detailed process of spraying are: evaporation concentration is to react 30～90min in 60～90 ℃ of evaporating pots, during keep vacuum tightness more than 500 mmhg, be less than 18% to material moisture; Carry out subsequently spray drying treatment, inlet temperature is controlled at 120～160 ℃, is dried to moisture and is less than 5%.
Embodiment 1
Use aforesaid method take inulin as raw material makes non-synthesis of oligonucleotides fructose, the Oranoleptic indicator of this non-synthesis of oligonucleotides fructose is specifically in Table 1.
Table 1
| Project | Index |
| Proterties | The unformed powder of white or micro-yellow |
| Smell | Oligofructose fragrant |
| Flavour | Sweet taste is soft salubrious |
The physical and chemical index of this non-synthesis of oligonucleotides fructose is specifically in Table 2.
Table 2
| Project | Index |
| Oligofructose total content (massfraction)/% >= | 95.0 |
| Moisture (massfraction)/%≤ | 5.0 |
| PH value | 4.5~7.0 |
| Electricity lead ash content/%≤ | 0.4 |
Compared to take sucrose as raw material production oligofructose, this method has obvious advantage aspect the oligofructose total content of finished product.
In the finished product of sucrose method, dextrose plus saccharose content is very high, and oligofructose only accounts for 55%～60% of total amount, and increasing refining and edulcoration link must raise the cost, and complex process, reacts wayward.
Oligofructose total content prepared by method of the present invention can reach more than 95%, can fully manifest the advantages such as the mineral absorptions such as its calorific value is low, promotion probiotics propagation, promotion calcium magnesium and unlikely carious tooth.
Claims (9)
1. a preparation method for non-synthesis of oligonucleotides fructose, is characterized in that, by following steps, is prepared from:
1) inulin solution is carried out to enzymolysis, enzymolysis product is filtered, obtain filtrate;
2) filtrate is decoloured processing;
3) filtrate after decolouring processing is carried out to flocculation treatment;
4), after flocculation filtration, spent ion exchange resin desalination, carries out removal of impurities, de-taste purifying;
5) above-mentioned product is carried out to evaporation concentration, spraying is dry, makes oligofructose.
2. according to the preparation method of non-synthesis of oligonucleotides fructose described in claim 1, it is characterized in that: in described step 1), the concentration of inulin solution is 40 ~ 60wt%.
3. according to the preparation method of non-synthesis of oligonucleotides fructose described in claim 1, it is characterized in that: the enzyme in described step 1) enzymolysis process is endoinulase, and the temperature of enzyme digestion reaction is 50～65 ℃, the reaction times is 18 ~ 22h.
4. according to the preparation method of non-synthesis of oligonucleotides fructose described in claim 3, it is characterized in that: the temperature of described enzyme digestion reaction is 55～59 ℃, the reaction times is 20h.
5. according to the preparation method of non-synthesis of oligonucleotides fructose described in claim 1, it is characterized in that described step 2) in decolouring process and to be specially: in filtrate, add gac, and the addition of the gac 0.1～5wt% that is reaction-ure mixture.
6. according to the preparation method of non-synthesis of oligonucleotides fructose described in claim 5, it is characterized in that, describedly by adding the gac processing of decolour, be specially: in temperature, be to be incubated 2～65min under 40～90 ℃ of conditions.
7. according to the preparation method of non-synthesis of oligonucleotides fructose described in claim 1, it is characterized in that, in described step 3), flocculation treatment is specially: adding the PAM flocculation agent of reaction-ure mixture 0.05～0.2wt%, is to react 2～65min at 45～75 ℃ in temperature under whipped state, after sedimentation, filters.
8. according to the preparation method of non-synthesis of oligonucleotides fructose described in claim 1, it is characterized in that, described step 4) intermediate ion exchange resin desalting treatment is specially: allow material by four resin filter beds of sun-male-female-the moon, carry out desalination successively, and controlling its flow velocity is 1～5BV/h, and initial charge temperature is 40～75 ℃.
9. according to the preparation method of non-synthesis of oligonucleotides fructose described in claim 1, it is characterized in that, in described step 5), the dry detailed process of evaporation concentration and spraying is: evaporation concentration is to react 30～90min in 60～90 ℃ of evaporating pots, keep during this time vacuum tightness more than 500 mmhg, be less than 18% to material moisture; Carry out subsequently spray drying treatment, inlet temperature is controlled at 120～160 ℃, is dried to moisture and is less than 5%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105177084A (en) * | 2015-10-29 | 2015-12-23 | 福建福大百特生物科技有限公司 | Method for producing fructooligosaccharides by fermenting inulase mutants |
| CN105801717A (en) * | 2016-03-30 | 2016-07-27 | 青海威德生物技术有限公司 | Method for producing fructo-oligosaccharide through membrane separation method |
| CN105861594A (en) * | 2016-05-23 | 2016-08-17 | 上海艾苛密进出口有限公司 | Preparation method of fructo-oligosaccharide |
| CN105950684A (en) * | 2016-07-01 | 2016-09-21 | 白银熙瑞生物工程有限公司 | Method for producing fructooligosaccharides by using jerusalem artichoke as raw material |
| CN106591264A (en) * | 2017-03-02 | 2017-04-26 | 福建省农业科学院农业工程技术研究所 | Endoglucanase promotion factor |
| CN109234336A (en) * | 2018-11-30 | 2019-01-18 | 中诺生物科技发展江苏有限公司 | A kind of method of dextrase enzymolysis inulin production oligofructose |
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| CN102732585A (en) * | 2011-12-25 | 2012-10-17 | 大兴安岭林格贝有机食品有限责任公司 | New method for purifying fructo oligosaccharide in chicory |
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| CN102732585A (en) * | 2011-12-25 | 2012-10-17 | 大兴安岭林格贝有机食品有限责任公司 | New method for purifying fructo oligosaccharide in chicory |
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| 游懿: "雪莲果低聚果糖提取分离及分析研究", 《中国优秀硕士学位论文全文数据库（工程科技I辑）》, no. 6, 15 June 2012 (2012-06-15), pages 023 - 344 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105177084A (en) * | 2015-10-29 | 2015-12-23 | 福建福大百特生物科技有限公司 | Method for producing fructooligosaccharides by fermenting inulase mutants |
| CN105801717A (en) * | 2016-03-30 | 2016-07-27 | 青海威德生物技术有限公司 | Method for producing fructo-oligosaccharide through membrane separation method |
| CN105861594A (en) * | 2016-05-23 | 2016-08-17 | 上海艾苛密进出口有限公司 | Preparation method of fructo-oligosaccharide |
| 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 |
| CN105950684A (en) * | 2016-07-01 | 2016-09-21 | 白银熙瑞生物工程有限公司 | Method for producing fructooligosaccharides by using jerusalem artichoke as raw material |
| CN106591264A (en) * | 2017-03-02 | 2017-04-26 | 福建省农业科学院农业工程技术研究所 | Endoglucanase promotion factor |
| CN109234336A (en) * | 2018-11-30 | 2019-01-18 | 中诺生物科技发展江苏有限公司 | A kind of method of dextrase enzymolysis inulin production oligofructose |
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