CN107245116A - A kind of method that utilization SMBC technology prepares high-purity polyfructosan - Google Patents
A kind of method that utilization SMBC technology prepares high-purity polyfructosan Download PDFInfo
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- CN107245116A CN107245116A CN201710638129.9A CN201710638129A CN107245116A CN 107245116 A CN107245116 A CN 107245116A CN 201710638129 A CN201710638129 A CN 201710638129A CN 107245116 A CN107245116 A CN 107245116A
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- polyfructosan
- purity
- area
- flow velocity
- inulin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0051—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Fructofuranans, e.g. beta-2,6-D-fructofuranan, i.e. levan; Derivatives thereof
- C08B37/0054—Inulin, i.e. beta-2,1-D-fructofuranan; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
Abstract
The invention discloses a kind of method that utilization SMBC technology prepares high-purity polyfructosan, this method comprises the following steps：(1) inulin crude extract decolourized, take off bitter, desalting processing, obtain inulin refined liquid；(2) the inulin refined liquid for obtaining step (1) adds moving bed imitation chromatogram separation facility and isolated and purified, using water as eluant, eluent, the Simulation moving bed includes I~IV area, each area includes 1~6 root chromatogram column, wherein Ith area, II area's chromatographic column filling strongly acidic cation-exchange, IIIth area, IV area's chromatographic column filling cationic molecule sieve；(3) obtained polyfructosan solution decompression is concentrated by evaporation, had both obtained high-purity polyfructosan.The purity of obtained polyfructosan is high, and total post effect is high, mobile phase consumption is few, it is possible to achieve operation serialization, improves the utilization rate of raw material, reduces production cost.
Description
Technical field
The invention belongs to polyfructosan preparing technical field, and in particular to one kind utilizes SMBC technology
The method for preparing high-purity polyfructosan.
Background technology
Witloof is composite family Cichorium herbaceos perennial, also known as European witloof, coffee grass or French sowthistle, is originated in
Europe, West Asia, the Central Asia and North America, the area such as NORTHWEST CHINA, North China and northeast are distributed.Chrysanthemum fragrant plant is of high nutritive value, disease-resistant
Insect pest and high yield, power of regeneration are strong, are a kind of high yield and high quality forage grass for having very much a potentiality to be exploited.Witloof fleshy root includes 70% or so
The inulin of (dry matter weight), can as inulin, FOS (FOS) and high fructose syrup raw materials for production.
Fructosyl series of products refer to the polysaccharide that D-Fructose is formed by connecting through β (1 → 2) glycosidic bond, and end often contains one
Glucosyl group, molecular formula is expressed as GFn, or Fm, and wherein G is terminal glucose unit (Glucose), and F represents fructose molecule
(Fructose), n or m then represent fructose units number.Generally, a glycosidic bond is a degree of polymerization (DP), the degree of polymerization of inulin
For 2~100, the degree of polymerization is polyfructosan when being more than 20, and (DP=2~9) are FOS during low polymerization degree, such as ketose,
Nystose, GF4, fruit fruit trisaccharide, fruit fruit tetrose, fruit fruit pentasaccharides etc., the ring-type constituted when two fructose are connected with each other
Disaccharides, then be difructose anhydride.
Mobile chromatogram (SMB) technology of simulation is more advanced means of purification both at home and abroad at present, be widely used in sugar alcohol,
Biological and medicine and other fields, this technology can realize serialization, the production of automation, in thermal sensitivity, isomer material
Separation on have distinctive feature.Domestic SMB technologies are at the early-stage, also in developing stage, at present only few several families
Company and university are studied, and achieve certain achievement.When carrying out SMB separation tests, it is necessary to real according to chromatogram is prepared
The result tested, subregion is designed on the basis of its data and initial parameter is calculated, and carries out technological parameter by testing adjustment
Optimization.SMB technologies can realize large-scale industrialization production, it is possible to achieve serialization, the control of automation, relatively prepare chromatogram
With larger advantage.But its input concentration of the mobile chromatographic technique of simulation of the prior art is low by general only 20%, product is more
The refractive power low 10% or so of Fructooligosaccharides causes the increase of concentrated cost.
The content of the invention
The technical problem to be solved in the invention is to provide a kind of many using SMBC technology preparation high-purity
The method of Fructooligosaccharides, to solve the problem of polyfructosan purity is not high in the prior art.
In order to solve the above technical problems, the present invention is adopted the following technical scheme that：
A kind of method that utilization SMBC technology prepares high-purity polyfructosan, this method includes following step
Suddenly：
(1) inulin crude extract decolourized, take off bitter, desalting processing, obtain inulin refined liquid；
(2) the inulin refined liquid for obtaining step (1) adds moving bed imitation chromatogram separation facility and isolated and purified, with
Water is eluant, eluent, and the Simulation moving bed includes I~IV area, and each area includes 1~6 root chromatogram column, wherein Ith area, IIth area
Chromatographic column fills strongly acidic cation-exchange, IIIth area, IV area's chromatographic column filling cationic molecule sieve；
The technological parameter isolated and purified is as follows：
Running temperature is 30 DEG C~60 DEG C, and pressure is 0.1~0.5Mpa, feeds 10~100mL/min of flow quantity, eluant, eluent
Flow be 50~150mL/min, set I areas flow velocity as 40cm/h~50cm/h, II areas flow velocity be 20cm/h~30cm/h,
III areas flow velocity is 50cm/h~65cm/h, and IV areas flow velocity is 10cm/h~20cm/h；
(3) obtained polyfructosan solution decompression is concentrated by evaporation, had both obtained high-purity polyfructosan.
In step (1), inulin crude extract decolourizes, the method for de- bitter, desalination is as follows：Inulin crude extract is passed sequentially through into activity
Charcoal, chitosan, cation macroreticular resin, NF membrane.
Preferably, described cation macroreticular resin is H103.
Preferably, described NF membrane is DL8040F.
Wherein, described strongly acidic cation-exchange is IR-120, Lewatit-100 or Dowex-50.
Preferably, the type of the cationic molecule sieve is Y type molecular sieve.
Preferably, the technological parameter isolated and purified is as follows：
Running temperature is 45 DEG C, and pressure is 0.15Mpa, feeds flow quantity 50mL/min, the flow of eluant, eluent is 50mL/
Min, sets I areas flow velocity as 45cm/h, and II areas flow velocity is 25cm/h, and III areas flow velocity is 55cm/h, and IV areas flow velocity is 14cm/h.
Wherein, described that concentration is evaporated under reduced pressure, its pressure is -0.098Mpa.
Beneficial effect：
The invention discloses a kind of method that utilization SMBC technology prepares high-purity polyfructosan, obtain
The purity of polyfructosan is high, and total post effect is high, mobile phase consumption is few, it is possible to achieve operation serialization, improves the utilization rate of raw material,
Reduce production cost.
Embodiment
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
Apply the content described by example and be merely to illustrate the present invention, without should be also without limitation on sheet described in detail in claims
Invention.
Embodiment 1：The preparation of inulin refined liquid.
Take the net fresh witloofs of 500g, peeling, grinding crushing；The witloof of crushing is added into the Tris-HCl containing pectase to delay
In fliud flushing, the concentration of the Tris-HCl buffer solutions is 1mol/L, and pH is 6.8, and the addition of pectase is 1000U/L, 35
3h is stirred under degree Celsius, extract solution is then heated to 100 DEG C, 5h is stirred；Inulin extract solution is filtered, inulin crude extract is obtained；
Inulin crude extract is decolourized, de- bitter, desalting processing, by inulin crude extract pass sequentially through activated carbon, chitosan,
Cation macroreticular resin, NF membrane, described cation macroreticular resin are H103, and described NF membrane is DL8040F, obtains chrysanthemum
Powder refined liquid.
Embodiment 2：
A kind of method that utilization SMBC technology prepares high-purity polyfructosan, this method includes following step
Suddenly：
Inulin refined liquid addition moving bed imitation chromatogram separation facility is isolated and purified, it is described using water as eluant, eluent
Simulation moving bed includes Ith area, IIth area, IIIth area, IVth area, and each area includes 6 root chromatogram columns, wherein Ith area, the chromatographic column filling of IIth area
IR-120 strongly acidic cation-exchanges, IIIth area, IV area's chromatographic column filling Y type molecular sieve；
The technological parameter isolated and purified is as follows：
Running temperature is 45 DEG C, and pressure is 0.15Mpa, feeds flow quantity 50mL/min, the flow of eluant, eluent is 50mL/
Min, sets I areas flow velocity as 45cm/h, and II areas flow velocity is 25cm/h, and III areas flow velocity is 55cm/h, and IV areas flow velocity is 14cm/h；
Obtained polyfructosan efflux solution decompression is concentrated by evaporation, the brix of polyfructosan brings up to 75 ° of Bx by 30 ° of Bx, both
To high-purity polyfructosan solution, wherein the content of polyfructosan is 97%, the polyfructosan degree of polymerization 80% concentrate on DP21~
30, polyfructosan extraction efficiency is 90%.
Embodiment 3：
Other conditions are same as Example 2, except that, adjust the running temperature of moving bed imitation chromatogram separation facility
For 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C.Detect content and the polymerization of polyfructosan flow export polyfructosan
Degree, testing result such as following table.
Influence of the temperature of table 1 to polyfructosan separative efficiency
Embodiment 4：Influence of the pressure to polyfructosan separative efficiency.
Other conditions are same as Example 2, except that, adjust the operating pressure of moving bed imitation chromatogram separation facility
For 0.1~0.5Mpa.Detect the content and the degree of polymerization of polyfructosan flow export polyfructosan, testing result such as following table.
Influence of the pressure of table 2 to polyfructosan separative efficiency
Embodiment 5：Influence of the strongly acidic cation-exchange to polyfructosan separative efficiency.
Other conditions are same as Example 2, except that, regulation moving bed imitation chromatogram separation facility strong-acid type sun from
The type of sub-exchange resin.Detect the content and the degree of polymerization of polyfructosan flow export polyfructosan, testing result such as following table.
Influence of the strongly acidic cation-exchange of table 3 to polyfructosan separative efficiency
Embodiment 6：Influence of the I areas flow velocity to polyfructosan separative efficiency.
Influence of the I areas flow velocity of table 4 to polyfructosan separative efficiency
Embodiment 7：Influence of the II areas flow velocity to polyfructosan separative efficiency.
Influence of the II areas flow velocity of table 5 to polyfructosan separative efficiency
Embodiment 8：Influence of the III areas flow velocity to polyfructosan separative efficiency.
Influence of the III areas flow velocity of table 6 to polyfructosan separative efficiency
Embodiment 9：Influence of the IV areas flow velocity to polyfructosan separative efficiency.
Influence of the IV areas flow velocity of table 7 to polyfructosan separative efficiency
Claims (8)
1. a kind of method that utilization SMBC technology prepares high-purity polyfructosan, it is characterised in that this method bag
Include following steps：
(1) inulin crude extract decolourized, take off bitter, desalting processing, obtain inulin refined liquid；
(2) the inulin refined liquid obtained step (1) adds moving bed imitation chromatogram separation facility and isolated and purified, using water as
Eluant, eluent, the Simulation moving bed includes I~IV area, and each area includes 1~6 root chromatogram column, wherein Ith area, II area's chromatogram
Post fills strongly acidic cation-exchange, IIIth area, IV area's chromatographic column filling cationic molecule sieve；
The technological parameter isolated and purified is as follows：
Running temperature is 30 DEG C~60 DEG C, and pressure is 0.1~0.5Mpa, feeds 10~100mL/min of flow quantity, the stream of eluant, eluent
Measure as 50~150mL/min, set I areas flow velocity as 40cm/h~50cm/h, II areas flow velocity is 20cm/h~30cm/h, III areas
Flow velocity is 50cm/h~65cm/h, and IV areas flow velocity is 10cm/h~20cm/h；
(3) obtained polyfructosan solution decompression is concentrated by evaporation, had both obtained high-purity polyfructosan.
2. the method for high-purity polyfructosan, its feature are prepared using SMBC technology according to claim 1
It is, in step (1), inulin crude extract decolourizes, the method for de- bitter, desalination is as follows：By inulin crude extract pass sequentially through activated carbon,
Chitosan, cation macroreticular resin, NF membrane.
3. the method for high-purity polyfructosan, its feature are prepared using SMBC technology according to claim 2
It is, described cation macroreticular resin is H103.
4. the method for high-purity polyfructosan, its feature are prepared using SMBC technology according to claim 2
It is, described NF membrane is DL8040F.
5. the method for high-purity polyfructosan, its feature are prepared using SMBC technology according to claim 1
It is, described strongly acidic cation-exchange is IR-120, Lewatit-100 or Dowex-50.
6. the method for high-purity polyfructosan, its feature are prepared using SMBC technology according to claim 1
It is, the type of the cationic molecule sieve is Y type molecular sieve.
7. the method for high-purity polyfructosan, its feature are prepared using SMBC technology according to claim 1
It is, the technological parameter isolated and purified is as follows：
Running temperature is 45 DEG C, and pressure is 0.15Mpa, feeds flow quantity 50mL/min, the flow of eluant, eluent is 50mL/min, if
I areas flow velocity is determined for 45cm/h, II areas flow velocity is 25cm/h, III areas flow velocity is 55cm/h, and IV areas flow velocity is 14cm/h.
8. the method for high-purity polyfructosan, its feature are prepared using SMBC technology according to claim 1
It is, described that concentration is evaporated under reduced pressure, its pressure is -0.098Mpa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111057166A (en) * | 2019-12-05 | 2020-04-24 | 晨光生物科技集团股份有限公司 | Method for preparing inulin |
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| EP2735573A1 (en) * | 2011-07-19 | 2014-05-28 | Nippon Beet Sugar Manufacturing Co. Ltd. | Method for producing inulin |
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| EP2735573A1 (en) * | 2011-07-19 | 2014-05-28 | Nippon Beet Sugar Manufacturing Co. Ltd. | Method for producing inulin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111057166A (en) * | 2019-12-05 | 2020-04-24 | 晨光生物科技集团股份有限公司 | Method for preparing inulin |
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Effective date of registration: 20200214 Address after: 518000 floor 28-03, Weisheng technology building, No. 9966, Shennan Avenue, Maling community, Yuehai street, Nanshan District, Shenzhen City, Guangdong Province Applicant after: Shenzhen hualikang fiber Biotechnology Co., Ltd Address before: 810000 Xining biological science and Technology Industrial Park, No. four, No. 10, Qinghai Applicant before: Dragon special Sugar Co. |
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