CN101367843B - Method for separating heteroside from tea saponin liquid to purify glucose and triterpene - Google Patents
Method for separating heteroside from tea saponin liquid to purify glucose and triterpene Download PDFInfo
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- CN101367843B CN101367843B CN2008101967115A CN200810196711A CN101367843B CN 101367843 B CN101367843 B CN 101367843B CN 2008101967115 A CN2008101967115 A CN 2008101967115A CN 200810196711 A CN200810196711 A CN 200810196711A CN 101367843 B CN101367843 B CN 101367843B
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- triterpene
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Abstract
The present invention relates to a method for separating out heterosugar from liquid tea saponin in order to purify glucose and triterpene, which belongs to the technical field of simulated moving bed chromatogram separation. Acidic calcium type chelate resin, which is specially used to absorb and separate out the glucose, the triterpene and the heterosugar, is first synthesized; and then, under an operation temperature between 60 DEG C and 80 DEG C and with water as eluent, a fixed bed, on which the acidic calcium type chelate resin is assembled, is adopted to use the simulated moving bed technology to separate out the heterosugar from the liquid tea saponin in order to purify the glucose and the triterpene, so that three types of components which are rich in the glucose, the triterpene and the heterosugar are respectively obtained. The method has the following advantages: the high-purity products of the glucose, the triterpene and the heterosugar can be produced; the production process is fully automated, labor intensity is low, and the production site is small; the production cost is low, and only 1 cubic meter to 4 cubic meters of water and a small amount of electricity are needed in the separation of liquid tea saponin per cubic meter; and the production process does not use any chemical and generate any pollution.
Description
Technical field
The present invention relates to from tea saponin liquid, separate the method for assorted sugar with purify glucose and triterpene, specifically, it relates to and ingeniously utilizes resin dedicated and simulated moving bed chromatography technology to separate the technology of assorted sugar with purifying and preparing high-purity glucose and triterpene from tea saponin liquid, belongs to the simulated moving bed chromatography separation technology field.
Background technology
Tea saponin is the class in the saponin, extensively is present in the plant of theaceae, by the pentacyclic triterpenoid saponin compounds that contains structure sugar and structure acid that extracts in the tea cake after all kinds of tea-seed, the tea seed oil expression.Its basic structure comprises sapogenin, sugared body, organic acid 3 parts.Therefore tea saponin removes in the tea saponin liquid that hydrolysis obtains and has corresponding sapogenin, sugared body portion (mainly containing glucose, pectinose, wood sugar, semi-lactosi and glucuronic acid etc.), organic acid part (mainly containing angelicic acid, tiglic acid, acetic acid and styracin etc.); Pigment, inorganic salt etc. are still arranged.
Summary of the invention
The objective of the invention is to seek a kind of method of from tea saponin liquid, separating assorted sugar, adopt the high efficiency chromatography separation method, to obtain high-quality glucose and triterpene product with purify glucose and triterpene.
Technical scheme of the present invention: a kind of method of from tea saponin liquid, separating assorted sugar, a, synthetic resins: the synthetic earlier acid calcium type resin that is used for special fractionation by adsorption glucose, triterpene and assorted sugar with purify glucose and triterpene; B, separation are purified: adopt the fixed bed that above-mentioned acid calcium type resin is housed to use simulated moving bed technology, separate the sugar of mixing with purify glucose and triterpene product from tea saponin liquid;
Wherein, acid calcium type resin as carrier, with calcium metal ion on its chelating, utilizes the avidity between acidic resins and the calcium metal ion with acid macroporous resin, on acid macroporous resin surface, and use linking agent to be fixed on the vector resin calcium metal ionic adsorption; Dosage of crosslinking agent is 2%～40% of an acid macroporous resin weight;
Metal Ca
2+The ionic type of service is can dissolved respective metal Ca under neutrality or alkaline condition
2+Ionic salt, metal Ca
2+The ionic amount is so that the resin chelating reaches 30% saturated amount～complete saturated amount.
Simulated moving bed technology: adopting above-mentioned acid calcium type resin in the moving bed imitation chromatogram separation facility is the stationary phase sorbent material, utilize the avidity difference between metal ion adsorbent and glucose, triterpene and the assorted sugar, realize the separation fully between glucose, triterpene and the assorted sugar; Simulation moving-bedly be connected in series the loop system that becomes head and the tail to connect by the chromatographic column that (does not contain 4) more than 4; Every root chromatogram column all has discharge port, opening for feed, circulation port, water-in; Adopt the computer auto-control mode to change the position of discharge port, opening for feed, circulation port, water-in, thereby realize charging, water inlet, preceding component discharging, the simultaneously continuous operation of back component discharging;
According to the position of opening for feed, discharge port and circulation port, all placed in-line chromatographic columns are divided into 5 districts in the system:
The I district: triterpene liquid exports to tea saponin liquid opening for feed, is called assorted sugar and extracts the district;
The II district: tea saponin liquid opening for feed is called glucose and extracts the district to the Glucose Liquid outlet;
The III district: Glucose Liquid exports to assorted liquid glucose outlet, is called and resolves the district;
The IV district: assorted liquid glucose exports to the eluting water import, is called the triterpene enrichment region;
The V district: the eluting water import is called the race way to the outlet of triterpene liquid;
Employing water is eluent, and separation temperature is 35 ℃～95 ℃, carries out charging, discharging operation continuously, obtains three class discharging components simultaneously, and the first kind is the component that is rich in glucose of glucose purity＞95%; Second class is the component that is rich in triterpene of triterpene purity＞91%; The 3rd class is the component that is rich in assorted sugar of assorted sugared purity＞74%.
Acid macroporous resin is selected acid polystyrene macroporous resin or acid polymethylmethacrylate class macroporous resin for use; Linking agent is the polyene-based linking agent.
The polyene-based linking agent is selected divinylbenzene, triethylene benzene or two propylene benzene for use.
Tea saponin liquid directly enters simulation moving-bed separation, obtains glucose, triterpene and assorted sugar product solution.
Separation temperature is 60 ℃～80 ℃.
Dosage of crosslinking agent is 6%～9% of a weight resin.
The resin of the present invention's preparation has higher physical stability than general commercial resin, and mill back rate of small round spheres＞99% is applicable to 90 ℃ of left and right sides prolonged operation temperature.This resin has very high resolution to glucose, triterpene and assorted sugar, general separable high concentration glucose liquid, triterpene liquid and the assorted liquid glucose that reaches mass concentration 20%.
Beneficial effect of the present invention: the 1. simulated moving bed chromatography technology that the present invention proposes a kind of pollution-free separation purify glucose, triterpene and assorted sugar product.Tea saponin liquid directly enters simulation moving-bed separation, obtains glucose, triterpene and assorted sugar product solution.Glucose, triterpene and assorted sugar have fabulous adsorption separation performance on this resin, realize the separation fully between glucose, triterpene and the assorted sugar substantially; 2. adopt the moving-bed continuous chromatography to separate resin utilization ratio height; 3. production process full-automation, labour intensity is low, and production site is little; 4. production cost is low, separates every cubic metre of tea saponin liquid, only needs 1 cubic metre～4 cubic metres water and a small amount of; 5. do not use any chemical in the production process, produce without any polluting.
Description of drawings
Fig. 1 tea saponin liquid technological process of production figure.
The zone chart of Fig. 2 chromatographic column.
Embodiment
Embodiment 1: synthetic resins
The synthetic earlier acid calcium type resin that is used for special fractionation by adsorption glucose, triterpene and assorted sugar;
Wherein, acid calcium type resin as carrier, with metal ion on its chelating, utilizes the avidity between glucose, triterpene and assorted sugar and the metal ion with acid macro porous crosslinking resin, and it is adsorbed on resin surface.The content of used linking agent in acid macroporous resin is 2%～40%, and the best is 6%～9%, and unit is a weight percentage.Acid calcium type resin with acid macroporous resin as carrier, with calcium metal ion on its chelating, utilize the avidity between acidic resins and the calcium metal ion, on acid macroporous resin surface, and use linking agent to be fixed on the vector resin calcium metal ionic adsorption; Dosage of crosslinking agent is 2%～40% of an acid macroporous resin weight;
Metal Ca
2+The ionic type of service is can dissolved respective metal Ca under neutrality or alkaline condition
2+Ionic salt, metal Ca
2+The ionic amount is so that the resin chelating reaches 30% saturated amount～complete saturated amount.
Embodiment 2: separate and purify
The fixed bed that above-mentioned acid calcium type resin is equipped with in employing uses simulated moving bed technology, separates from tea saponin liquid and purifies, and obtains purified glucose, triterpene and assorted sugar product;
Simulated moving bed technology: adopting above-mentioned acid calcium type resin in the moving bed imitation chromatogram separation facility is the stationary phase sorbent material, utilize the avidity difference between macromole metal absorbent and glucose, triterpene and the assorted sugar, realize the separation fully between glucose, triterpene and the assorted sugar; Employing water is eluent, and separation temperature is 35 ℃～95 ℃, and the optimal separation temperature is 60 ℃～80 ℃, carries out charging, discharging operation continuously, obtains three class discharging components simultaneously, and the first kind is for being rich in the component of glucose (glucose purity＞95%); Second class is for being rich in the component of triterpene (triterpene purity＞91%); The 3rd class is for being rich in the component of assorted sugar (assorted sugared purity＞74%).
Macroporous resin is acid polystyrene macroporous resin or polymethylmethacrylate class macroporous resin; Linking agent is the polyene-based linking agent, as divinylbenzene or triethylene benzene or two propylene benzene etc.
Tea saponin liquid directly enters simulation moving-bed separation, obtains glucose, triterpene and assorted sugar product solution.Simulation moving-bed chromatographic column is not connected in series by (not containing 4) more than 4, the loop system that becomes head and the tail to connect; Every root chromatogram column all has discharge port, opening for feed, circulation port, water-in; Adopt the computer auto-control mode to change the position of discharge port, opening for feed, circulation port, water-in, thereby realize charging, water inlet, preceding component discharging, the simultaneously continuous operation of back component discharging.
According to the position of feed inlet and outlet and circulation port, all placed in-line chromatographic columns are divided into 5 districts in the system:
The I district: triterpene liquid exports to tea saponin liquid opening for feed, is called assorted sugar and extracts the district.
The II district: tea saponin liquid opening for feed is called glucose and extracts the district to the Glucose Liquid outlet.
The III district: Glucose Liquid exports to assorted liquid glucose outlet, is called and resolves the district.
The IV district: assorted liquid glucose exports to the eluting water inlet, is called the triterpene enrichment region.
The V district: enter the mouth triterpene liquid outlet of eluting water is called the race way.
Further introduce technology of the present invention below in conjunction with embodiment.
Feeding liquid is a tea saponin liquid, its concentration is about 60%, wherein glucose 10.4%, triterpene 29.5%, assorted sugar 46.2%, pass through this liquid simulation moving-bed, simulation moving-bed operational condition is as follows: 75 ℃ of separation temperatures, and system pressure 1.1Mpa, the feed liquid inlet amount is 1L/h, the eluting water inlet amount is 3.5L/h, and charging reached balance after 24 hours.The discharging situation that obtains is as follows:
1) glucose moiety: concentration is about 34%, glucose purity 95%, triterpene purity 3%, assorted sugared purity 2%.
2) triterpene part: concentration is about 29%, triterpene purity 91%, glucose purity 1%, assorted sugar 8%.
3) assorted sugar moieties: concentration is about 14%, assorted sugared purity 74%, glucose purity 6%, triterpene purity 20%.
Claims (6)
1. a method of separating assorted sugar with purify glucose and triterpene from tea saponin liquid is characterized in that a, synthetic resins: the synthetic earlier acid calcium type resin that is used for special fractionation by adsorption glucose, triterpene and assorted sugar; B, separation are purified: adopt the fixed bed that above-mentioned acid calcium type resin is housed to use simulated moving bed technology, separate the sugar of mixing with purify glucose and triterpene product from tea saponin liquid;
Wherein, acid calcium type resin as carrier, with calcium metal ion on its chelating, utilizes the avidity between acidic resins and the calcium metal ion with acid macroporous resin, on acid macroporous resin surface, and use linking agent to be fixed on the vector resin calcium metal ionic adsorption; Dosage of crosslinking agent is 2%～40% of an acid macroporous resin weight;
Metal Ca
2+The ionic type of service is can dissolved respective metal Ca under neutrality or alkaline condition
2+Ionic salt, metal Ca
2+The ionic amount is so that the resin chelating reaches 30% saturated amount～complete saturated amount;
Simulated moving bed technology: adopting above-mentioned acid calcium type resin in the moving bed imitation chromatogram separation facility is the stationary phase sorbent material, utilize the avidity difference between metal ion adsorbent and glucose, triterpene and the assorted sugar, realize the separation fully between glucose, triterpene and the assorted sugar; Simulation moving-bed the chromatographic column that does not contain 4 is connected in series by more than 4, the loop system that becomes head and the tail to connect; Every root chromatogram column all has discharge port, opening for feed, circulation port, water-in; Adopt the computer auto-control mode to change the position of discharge port, opening for feed, circulation port, water-in, thereby realize charging, water inlet, preceding component discharging, the simultaneously continuous operation of back component discharging;
According to the position of opening for feed, discharge port and circulation port, all placed in-line chromatographic columns are divided into 5 districts in the system:
The I district: triterpene liquid exports to tea saponin liquid opening for feed, is called assorted sugar and extracts the district;
The II district: tea saponin liquid opening for feed is called glucose and extracts the district to the Glucose Liquid outlet;
The III district: Glucose Liquid exports to assorted liquid glucose outlet, is called and resolves the district;
The IV district: assorted liquid glucose exports to the eluting water import, is called the triterpene enrichment region;
The V district: the eluting water import is called the race way to the outlet of triterpene liquid;
Employing water is eluent, and separation temperature is 35 ℃～95 ℃, carries out charging, discharging operation continuously, obtains three class discharging components simultaneously, and the first kind is the component that is rich in glucose of glucose purity＞95%; Second class is the component that is rich in triterpene of triterpene purity＞91%; The 3rd class is the component that is rich in assorted sugar of assorted sugared purity＞74%.
2. according to the described method of from tea saponin liquid, separating assorted sugar of claim 1, it is characterized in that acid macroporous resin is selected acid polystyrene macroporous resin or acid polymethylmethacrylate class macroporous resin for use with purify glucose and triterpene; Linking agent is the polyene-based linking agent.
3. according to the described method of from tea saponin liquid, separating assorted sugar of claim 2, it is characterized in that the polyene-based linking agent is selected divinylbenzene, triethylene benzene or two propylene benzene for use with purify glucose and triterpene.
4. according to the described method of from tea saponin liquid, separating assorted sugar of claim 1, it is characterized in that tea saponin liquid directly enters simulation moving-bed separation, obtain glucose, triterpene and assorted sugar product solution with purify glucose and triterpene.
5. according to the described method of from tea saponin liquid, separating assorted sugar of claim 1, it is characterized in that separation temperature is 60 ℃～80 ℃ with purify glucose and triterpene.
6. according to the described method of from tea saponin liquid, separating assorted sugar of claim 1, it is characterized in that dosage of crosslinking agent is 6%～9% of a weight resin with purify glucose and triterpene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101967115A CN101367843B (en) | 2008-09-17 | 2008-09-17 | Method for separating heteroside from tea saponin liquid to purify glucose and triterpene |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101967115A CN101367843B (en) | 2008-09-17 | 2008-09-17 | Method for separating heteroside from tea saponin liquid to purify glucose and triterpene |
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| Publication Number | Publication Date |
|---|---|
| CN101367843A CN101367843A (en) | 2009-02-18 |
| CN101367843B true CN101367843B (en) | 2010-10-06 |
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|---|---|---|---|---|
| CN103265663B (en) * | 2013-05-30 | 2015-04-22 | 广西民族大学 | Glucosyl containing rosinyl macroporous resin and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6451123B1 (en) * | 1999-01-14 | 2002-09-17 | Board Of Supervisors Of Louisiana State University And Agricultural And Mechanical College | Process for the separation of sugars |
| CN1528769A (en) * | 2003-09-28 | 2004-09-15 | 南宁市化工研究设计院 | Process for separating mannitose and glucose by analog moving bed |
| CN1715423A (en) * | 2005-07-01 | 2006-01-04 | 江南大学 | Method for extracting high purity glucose and functional oligose from crystalline glucose mother liquid |
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2008
- 2008-09-17 CN CN2008101967115A patent/CN101367843B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6451123B1 (en) * | 1999-01-14 | 2002-09-17 | Board Of Supervisors Of Louisiana State University And Agricultural And Mechanical College | Process for the separation of sugars |
| CN1528769A (en) * | 2003-09-28 | 2004-09-15 | 南宁市化工研究设计院 | Process for separating mannitose and glucose by analog moving bed |
| CN1715423A (en) * | 2005-07-01 | 2006-01-04 | 江南大学 | Method for extracting high purity glucose and functional oligose from crystalline glucose mother liquid |
Non-Patent Citations (1)
| Title |
|---|
| JP特开平9-145702A 1997.06.06 |
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Granted publication date: 20101006 Termination date: 20130917 |