CN105194904A - Continuous chromatographic separation and purification system for separating sugar in inulin - Google Patents
Continuous chromatographic separation and purification system for separating sugar in inulin Download PDFInfo
- Publication number
- CN105194904A CN105194904A CN201510560169.7A CN201510560169A CN105194904A CN 105194904 A CN105194904 A CN 105194904A CN 201510560169 A CN201510560169 A CN 201510560169A CN 105194904 A CN105194904 A CN 105194904A
- Authority
- CN
- China
- Prior art keywords
- inulin
- purification system
- separating
- sugar
- zone
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention provides a continuous chromatographic separation and purification system for separating sugar in inulin. A plurality of separation units which are connected together in series are driven by a turntable to rotate, and when the turntable rotates a circle, under the action of cation exchange resin filled in the separation units, fructo-oligosaccharide flows out of an elution area, polyfructose flows out of a separation area, and recycled water flows out of a concentration area. In such a manner, an inulin solution is separated and purified, so that links of exchange, washing, recycling, leaching and the like in an original fixed bed are integrated in the same system to achieve a better separation and purification effect.
Description
Technical field
The present invention relates to fluid separation applications technical field of purification, particularly relate to a kind of continuous chromatography separation and purification system for separating of sugar in inulin.
Background technology
Inulin is that fructose molecule connects with β-(2-1) glycosidic bond, the fructan mixt that end ends up with a glucose molecule.At present, inulin is mainly derived from jerusalem artichoke and witloof.The fructose units degree of polymerization of natural inulin is generally 2-60, and average degree of polymerization is about 10.
In inulin, the levulan of degree of polymerization 2-9 is commonly referred to as FOS, and FOS content in inulin is generally 5-35%.FOS is a kind of natural active matter, has regulating intestinal canal flora, propagation Bifidobacterium, keeps gut flora balance, promotes that stomach absorbs, the novel sweetener of the health cares such as anti-caries tooth.
Polyfructosan is in fact long-chain inulin, is to be removed by the short chain moieties in natural inulin, and average degree of polymerization controls 23 or more.Polyfructosan is a kind of natural fat substitute, when it is dissolved completely in water, can form a kind of creamy texture, is easy to and food blending, can be used to replace fat and provides a kind of level and smooth smectic mouthfeel and balance plentiful fragrance.Polyfructosan shows extraordinary stability in the technique of Strong shear power, is more suitable for applying in the food industry.
When fixed-bed intermittent formula separating oligomeric fructose and polyfructosan, whole bed only has a small amount of resin of mass-transfer zone in work, and most of resin is in inactive idle and wait state, there is the drawback that the utilization rate of resin is low; Simultaneously a large amount of materials or regenerative agent need through or soak the resin of inactivation, cause the pollution to resin.The cycle run in addition is long, and pipeline and the valve of connection are many, complex operation; Resin utilization ratio is low, causes the resin bed that separation process needs are very large, a large amount of wash waters; Not only floor space is large, product purity, concentration and yield are low, and acid-base waste fluid discharge capacity is large, and environmental pollution is serious.
Summary of the invention
Have in view of that, the invention provides a kind of continuous chromatography separation and purification system for separating of sugar in inulin, effectively to solve prior art Problems existing.
For separating of a continuous chromatography separation and purification system for sugar in inulin, comprising:
Rotating disk, rotatably rotates;
Separation assembly, be fixed on described rotating disk, described separation assembly comprises 20 separative elements, described separative element is annularly connected successively by pipeline and is fixed on described rotating disk, wherein, the described separative element in first, each region also offers charging aperture, is filled with cationic ion-exchange resin in described separative element, and described cationic ion-exchange resin is the K type resin of DTF-01 after supersaturation KCl solution makes the transition;
20 described separative elements are equally divided into: elution zone, adsorption zone, Disengagement zone and enrichment region, through the inulin solution that the Disengagement zone charging aperture of described separative element enters, enter successively again in described adsorption zone, elution zone and enrichment region to complete and once circulate, when described turntable rotation one week, FOS is flowed out through described elution zone, flow out polyfructosan through described Disengagement zone, flow out recycled water through described enrichment region.
In certain embodiments, the direction of rotation of described separative element is contrary with the flow direction of the eluent of its inside.
In certain embodiments, described separative element comprises resin column, described resin column ringwise shape is arranged on described rotating disk, the centre of described resin column arranges stiff end and round end, the notch pipeline of described round end is connected to next resin column, and the notch of described stiff end is connected with the material pipe of inlet and outlet system.
In certain embodiments, the concentration of described inulin solution is 10 ~ 300g/L.
In certain embodiments, the flow velocity V1 of described elution zone is 45-60ml/min, and the flow velocity V2 of described adsorption zone is 30-50ml/min, and the flow velocity V3 of described Disengagement zone is 30-50ml/min, and the flow velocity V4 of described enrichment region is 35-55ml/min.
In certain embodiments, described rotating disk circulation timei is 1800 ~ 9000s, and the described rotating disk intercycle time is 100 ~ 480s.
The present invention adopts technique scheme to have following beneficial effect:
A kind of continuous chromatography separation and purification system for separating of sugar in inulin that the invention provides, rotated by the some separative elements be cascaded of driven by rotary disc, under the cationic ion-exchange resin effect of filling in described separative element, when described turntable rotation one week, FOS is flowed out through described elution zone, polyfructosan is flowed out through described Disengagement zone, recycled water is flowed out through described enrichment region, achieve the separation and purification of inulin solution like this, thus by the exchange in original fixed bed, washing, regeneration, the links such as drip washing are incorporated in same system, achieve better separation and purification effect.
In addition, the continuous chromatography separation and purification system for separating of sugar in inulin provided by the invention, changes into continuous print process by the mode of interval, not only can improve utilization rate and the process recovery ratio of resin, also substantially increase production efficiency.
Accompanying drawing explanation
Fig. 1 is the structural representation of the continuous chromatography separation and purification system for separating of sugar in inulin provided by the invention;
Fig. 2 is the structural representation of the separative element of the continuous chromatography separation and purification system for separating of sugar in inulin provided by the invention;
Fig. 3 is the TLC analysis chart of the separating effect of each embodiment.
Detailed description of the invention
For the ease of understanding the present invention, below with reference to relevant drawings, the present invention is described more fully.Better embodiment of the present invention is given in accompanying drawing.These are only the preferred embodiments of the present invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention and accompanying drawing content to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Unless otherwise defined, all technology used herein and scientific terminology are identical with belonging to the implication that those skilled in the art of the present invention understand usually.The object of term used in the description of the invention herein just in order to describe concrete embodiment, is not intended to be restriction the present invention.Term as used herein " and/or " comprise arbitrary and all combinations of one or more relevant Listed Items.
Refer to Fig. 1, a kind of continuous chromatography separation and purification system 100 for separating of sugar in inulin that the embodiment of the present invention provides, comprising: rotating disk (not shown) and separation assembly 110.
Wherein, rotating disk, rotatably rotates.Preferably, the time that described rotating disk circulates one week is 1800 ~ 9000s, and the interval time after described rotating disk circulates one week is 100 ~ 480s.
Preferably, rotating disk is connected with drive motors, and under the driving of described drive motors, described rotating disk rotatably rotates.
Separation assembly 110, is fixed on described rotating disk, and described separation assembly 110 comprises some separative elements 111, and some described separative elements 111 are sequentially connected in series by pipeline, are filled with cationic ion-exchange resin in described separative element.
Preferably, described cationic ion-exchange resin is the K type resin of DTF-01 after supersaturation KCl solution makes the transition.
Preferably, the described direction of rotation of separative element 111 is contrary with the flow direction of the eluent of its inside.Be appreciated that flow direction due to the eluent of separative element 111 inside is contrary with the direction of rotation of described separative element 111 thus ion-exchange can be carried out better, improve purification efficiency.
Preferably, described separative element 111 is 20, and described separative element 111 is annularly connected and is fixed on described rotating disk.
Particularly, described separative element 111 comprises resin column 112, described cationic ion-exchange resin is built in described resin column 112, described resin column ringwise shape is arranged on described rotating disk, the centre of described resin column 112 arranges stiff end a and round end b, the notch (not shown) pipeline of described round end b is connected to the stiff end a of next resin column, and the notch (not shown) of described stiff end a is connected with the material pipe of inlet and outlet system c.Be appreciated that separative element 111 is by being designed to said structure, thus improve exchange effect.
Be appreciated that, different according to the function of separative element 111,20 described separative elements are equally divided into: elution zone, adsorption zone, Disengagement zone and enrichment region, through the inulin solution that 3 differentiation abscission zone charging apertures of described separative element 111 enter, to enter successively again in 2 district's adsorption zones, 1 elution zone, district and 4 district's enrichment regions thus complete and once circulate, when described turntable rotation one week, flow out FOS through described elution zone, flow out polyfructosan through described Disengagement zone, flow out recycled water through described enrichment region.
Preferably, the concentration of described inulin solution is 10 ~ 300g/L.
Be appreciated that inulin is a kind of preferred embodiment provided by the invention, other solution of above-mentioned separation and purification systematic position in reality, can also be adopted.
Further, the flow velocity V1 of described elution zone is 45-60ml/min, and the flow velocity V2 of described adsorption zone is 30-50ml/min, and the flow velocity V3 of described Disengagement zone is 30-50ml/min, and the flow velocity V4 of described enrichment region is 35-55ml/min.
A kind of continuous chromatography separation and purification system for separating of sugar in inulin that the invention provides, rotated by the some separative elements be cascaded of driven by rotary disc, under the cationic ion-exchange resin effect of filling in described separative element, when described turntable rotation one week, FOS is flowed out through described elution zone, polyfructosan is flowed out through described Disengagement zone, recycled water is flowed out through described enrichment region, achieve the separation and purification of inulin solution like this, thus by the exchange in original fixed bed, washing, regeneration, the links such as drip washing are incorporated in same system, achieve better separation and purification effect.
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1:
A. prepare the inulin solution 10L of 100g/L, connect instrument by operation rules, 1 district's access 75L pure water, accesses 5L pure water in 2nd district and 3rd district;
B. set the experiment parameter of panel and pump discharge, press " initial point sought by rotating disk " button, clean up time, the Feed flow rate of peristaltic pump is set to 5ml/min simultaneously;
| Position | Setting flow velocity (ml/min) |
| No. 1 mouth (1st district) | 60 |
| No. 6 mouths (2nd district) | 44 |
| No. 11 mouths (3rd district) | 49 |
| No. 16 mouths (4th district) | 40 |
C. open the switch of pump, press " rotating disk startup " button, ensure that normal operation do not revealed by instrument afterwards;
D. test operation to sample after 24 hours, analyzed by institute's sample thief point TLC plate, 1st district, 3 district's sampling results are shown in Fig. 3 the 2nd, 3 road thin-layer chromatography result respectively.
Embodiment 2:
A. prepare the inulin solution 10L of 200g/L, connect instrument according to flow chart, 1 district's access 75L pure water, accesses 5L pure water in 2nd district and 3rd district;
B. set the experiment parameter of panel and pump discharge, press " initial point sought by rotating disk " button, clean up time, the Feed flow rate of peristaltic pump is set to 4ml/min simultaneously
| Position | Setting flow velocity (ml/min) |
| No. 1 mouth (1st district) | 50 |
| No. 6 mouths (2nd district) | 42 |
| No. 11 mouths (3rd district) | 46 |
| No. 16 mouths (4th district) | 36 |
C. open the switch of pump, press " rotating disk startup " button, ensure that normal operation do not revealed by instrument afterwards;
D. test operation to sample after 24 hours, analyzed by institute's sample thief point TLC plate, 1st district, 3 district's sampling results are shown in Fig. 3 the 4th, 5 road thin-layer chromatography result respectively.
Embodiment 3:
A. prepare the inulin solution 10L of 200g/L, connect instrument according to flow chart, 1 district's access 75L pure water, accesses 5L pure water in 2nd district and 3rd district;
B. set the experiment parameter of panel and pump discharge, press " initial point sought by rotating disk " button, clean up time, the Feed flow rate of peristaltic pump is set to 5ml/min simultaneously;
| Position | Setting flow velocity (ml/min) |
| No. 1 mouth (1st district) | 50 |
| No. 6 mouths (2nd district) | 39 |
| No. 11 mouths (3rd district) | 44 |
| No. 16 mouths (4th district) | 40 |
C. open the switch of pump, press " rotating disk startup " button, ensure that normal operation do not revealed by instrument afterwards;
D. test operation to sample after 24 hours, analyzed by institute's sample thief point TLC plate, 1st district, 3 district's sampling results are shown in Fig. 3 the 7th, 6 road thin-layer chromatography result respectively.
Referring to Fig. 3 is that each band is from left to right followed successively by: 1 road is inulin; 2 roads are 1st district sampling in embodiment 1; 3 roads are 3rd district sampling in embodiment 1; 4 roads are 1st district sampling in embodiment 2; 5 roads are 3rd district sampling in embodiment 2; 6 roads are 3rd district sampling in embodiment 3; 7 roads are 1st district sampling in embodiment 3; 8 roads are inulin; 9 roads are FOS standard items; 10 roads are glucose; 11 roads are fructose; 12 roads are sucrose.
As seen from Figure 3, through isolation and purification method of the present invention, 1 region effluent of equipment is FOS, and 3 region effluents are polyfructosan.Therefore, The inventive method achieves FOS in inulin to be separated with the effective of polyfructosan.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (7)
1., for separating of a continuous chromatography separation and purification system for sugar in inulin, it is characterized in that, comprising:
Rotating disk, rotatably rotates;
Separation assembly, be fixed on described rotating disk, described separation assembly comprises 20 separative elements, described separative element is annularly connected successively by pipeline and is fixed on described rotating disk, wherein, be filled with cationic ion-exchange resin in described separative element, described cationic ion-exchange resin is the K type resin of DTF-01 after supersaturation KCl solution makes the transition;
20 described separative elements are equally divided into: elution zone, adsorption zone, Disengagement zone and enrichment region, through the inulin solution that the Disengagement zone charging aperture of described separative element enters, enter successively again in described adsorption zone, elution zone and enrichment region to complete and once circulate, when described turntable rotation one week, FOS is flowed out through described elution zone, flow out polyfructosan through described Disengagement zone, flow out recycled water through described enrichment region.
2. the continuous chromatography separation and purification system for separating of sugar in inulin according to claim 1, it is characterized in that, the direction of rotation of described separative element is contrary with the flow direction of the eluent of its inside.
3. the continuous chromatography separation and purification system for separating of sugar in inulin according to claim 2, it is characterized in that, described separative element comprises resin column, described cationic ion-exchange resin is built in described resin column, described resin column ringwise shape is arranged on described rotating disk, the centre of described resin column arranges stiff end and round end, and the notch pipeline of described round end connects next resin column, and the notch of described stiff end is connected with the material pipe of inlet and outlet system.
4. the continuous chromatography separation and purification system for separating of sugar in inulin according to claim 1, is characterized in that, the concentration of described inulin solution is 10 ~ 300g/L.
5. the continuous chromatography separation and purification system for separating of sugar in inulin according to claim 1, it is characterized in that, the flow velocity V1 of described elution zone is 45-60ml/min, the flow velocity V2 of described adsorption zone is 30-50ml/min, the flow velocity V3 of described Disengagement zone is 30-50ml/min, and the flow velocity V4 of described enrichment region is 35-55ml/min.
6. the continuous chromatography separation and purification system for separating of sugar in inulin according to claim 1, is characterized in that, described rotating disk circulation timei is 1800 ~ 9000s, and the described rotating disk intercycle time is 100 ~ 480s.
7. the continuous chromatography separation and purification system for separating of sugar in inulin according to claim 1, is characterized in that, described cationic ion-exchange resin is the K type resin of DTF-01 after supersaturation KCl solution makes the transition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510560169.7A CN105194904B (en) | 2015-09-06 | 2015-09-06 | Continuous chromatographic separation and purification system for separating sugar in inulin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510560169.7A CN105194904B (en) | 2015-09-06 | 2015-09-06 | Continuous chromatographic separation and purification system for separating sugar in inulin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105194904A true CN105194904A (en) | 2015-12-30 |
| CN105194904B CN105194904B (en) | 2017-01-25 |
Family
ID=54943065
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510560169.7A Active CN105194904B (en) | 2015-09-06 | 2015-09-06 | Continuous chromatographic separation and purification system for separating sugar in inulin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105194904B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105797428A (en) * | 2016-03-18 | 2016-07-27 | 中国科学院青海盐湖研究所 | Device and method for removing impurities in high-lithium solution |
| CN106706813A (en) * | 2017-02-07 | 2017-05-24 | 中检科（北京）测试技术有限公司 | Ion chromatography determination method for content of polyfructose in food and milk powder for infants and young children |
| CN110465114A (en) * | 2019-08-23 | 2019-11-19 | 内蒙古金达威药业有限公司 | A kind of Simulation moving bed continuous chromatography chromatographic system and its application and the method for purifying Co-Q10 |
| CN112973806A (en) * | 2021-02-09 | 2021-06-18 | 珠海高新区维得力生物工程有限公司 | Chromatographic separation filler applied to fructo-oligosaccharide, preparation process and chromatographic separation device |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6106724A (en) * | 1997-07-08 | 2000-08-22 | Uop Llc | Process for separating chiral compounds using a unimodal large pore silica as the support |
| CN101177716A (en) * | 2007-12-12 | 2008-05-14 | 江南大学 | Method for separating and purifying glucose, fructose and oligomeric polysaccharide from high fructose syrup |
| BRPI1002906A2 (en) * | 2010-08-11 | 2012-05-29 | Solange Vandresen | inulin / tubers fos discoloration and phenolic recovery by sorption process |
| CN103642876A (en) * | 2013-12-12 | 2014-03-19 | 保龄宝生物股份有限公司 | Method for preparing high-purity chicory and helianthus tuberosus fructo-oligosaccharide in coproduction of polyfructosan |
-
2015
- 2015-09-06 CN CN201510560169.7A patent/CN105194904B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6106724A (en) * | 1997-07-08 | 2000-08-22 | Uop Llc | Process for separating chiral compounds using a unimodal large pore silica as the support |
| CN101177716A (en) * | 2007-12-12 | 2008-05-14 | 江南大学 | Method for separating and purifying glucose, fructose and oligomeric polysaccharide from high fructose syrup |
| BRPI1002906A2 (en) * | 2010-08-11 | 2012-05-29 | Solange Vandresen | inulin / tubers fos discoloration and phenolic recovery by sorption process |
| CN103642876A (en) * | 2013-12-12 | 2014-03-19 | 保龄宝生物股份有限公司 | Method for preparing high-purity chicory and helianthus tuberosus fructo-oligosaccharide in coproduction of polyfructosan |
Non-Patent Citations (3)
| Title |
|---|
| ELOY CUSIMAMANI FERNÁNDEZ ET AL.: "Impact of yacon landraces cultivated in the Czech Republic and their ploidy on the short- and long-chain fructooligosaccharides content in tuberous roots", 《LWT - FOOD SCIENCE AND TECHNOLOGY》 * |
| 熊结青: "连续式色谱分离系统分离果糖的应用研究", 《中国优秀硕士学位论文全文数据库》 * |
| 王建华等: "离子色谱法测定菊芋和菊苣中菊糖", 《理化检验-化学分册》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105797428A (en) * | 2016-03-18 | 2016-07-27 | 中国科学院青海盐湖研究所 | Device and method for removing impurities in high-lithium solution |
| CN105797428B (en) * | 2016-03-18 | 2018-06-01 | 中国科学院青海盐湖研究所 | A kind of device and method for removing the impurity in high lithium solution |
| CN106706813A (en) * | 2017-02-07 | 2017-05-24 | 中检科（北京）测试技术有限公司 | Ion chromatography determination method for content of polyfructose in food and milk powder for infants and young children |
| CN110465114A (en) * | 2019-08-23 | 2019-11-19 | 内蒙古金达威药业有限公司 | A kind of Simulation moving bed continuous chromatography chromatographic system and its application and the method for purifying Co-Q10 |
| CN110465114B (en) * | 2019-08-23 | 2021-08-20 | 内蒙古金达威药业有限公司 | Simulated moving bed continuous chromatography chromatographic system, application thereof and method for purifying coenzyme Q10 |
| CN112973806A (en) * | 2021-02-09 | 2021-06-18 | 珠海高新区维得力生物工程有限公司 | Chromatographic separation filler applied to fructo-oligosaccharide, preparation process and chromatographic separation device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105194904B (en) | 2017-01-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105194904A (en) | Continuous chromatographic separation and purification system for separating sugar in inulin | |
| JP5133872B2 (en) | Method and apparatus for chromatographic purification | |
| Liu et al. | A simple method for the simultaneous decoloration and deproteinization of crude levan extract from Paenibacillus polymyxa EJS-3 by macroporous resin | |
| IE891580L (en) | Method for the recovery of betaine from molasses | |
| CZ295294B6 (en) | Method for fractionation of a solution by a chromatographic simulated moving bed process | |
| Van Walsem et al. | Simulated moving bed in the production of lysine | |
| CN111269276B (en) | Production method for separating acarbose and impurities | |
| Achaerandio et al. | Continuous vinegar decolorization with exchange resins | |
| JP6013639B1 (en) | Chromatographic separation method and apparatus for separating multiple components into three or more fractions | |
| CN101899486A (en) | Method for separating and purifying oligo-xylose by using simulated moving bed | |
| CN102671427A (en) | Simulated moving bed for chromatography device | |
| CN104878056B (en) | A method of producing high-purity fructo oligosaccharides | |
| CN109836479B (en) | Method for separating and purifying FMD inactivated virus antigen by using simulated fluid bed | |
| US6395179B1 (en) | Thermally-managed separation and dewatering processes for recovering acid products | |
| WO1992009352A1 (en) | Method of and device for counter-flow separation of mixture | |
| CN109021040B (en) | Continuous chromatographic separation and purification method of geniposide | |
| CN104815460B (en) | A kind of continous way adsorption plant | |
| CN210278337U (en) | Chromatographic separation system | |
| JP3783756B2 (en) | Desalination method | |
| CN1528769A (en) | Process for separating mannitose and glucose by analog moving bed | |
| JP2740780B2 (en) | Simulated moving bed equipment | |
| CN113769794A (en) | Ion exchange system and method for continuously removing impurities in citicoline sodium | |
| CN204675854U (en) | A kind of continous way adsorption unit | |
| JPH0724725B2 (en) | Liquid chromatographic separation device for three-component separation | |
| JPH0779927B2 (en) | Pseudo moving bed type liquid chromatographic oligosaccharide separator |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |