CN104713973A - Two-dimensional preparative chromatography instrument system having online enrichment function, and applications thereof - Google Patents
Two-dimensional preparative chromatography instrument system having online enrichment function, and applications thereof Download PDFInfo
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Abstract
The present invention relates to a two-dimensional preparative chromatography instrument system having the online enrichment function, and applications thereof. The system comprises a chromatography flow channel switching valve, a chromatography column, a solvent pump and a detector. According to the present invention, a trapping column collects a first-dimensional chromatography effluent component through valve switching and mobile phase dilution, and the trapped component is introduced into a second-dimensional preparative column through valve switching and mobile phase elution so as to achieve two-dimensional chromatography separation; the instrument system can perform two-dimensional separation, and the sample and the one-dimensional separation component are effectively retained and enriched through the trapping column interface, such that the column efficiency loss is low, and the two-dimensional separation effect is ensured; and the instrument system can enlargedly perform multiple circulation separations and multidimensional separation, and the separation effect can not be decreased along with the increasing sample volume and the increasing separation frequency. In addition, the instrument system further has the function of the concentration recovery on the finally-separated product so as to simplify the sample drying process, such that the degeneration of the sample during the heating drying process is easily be avoided.
Description
Technical field
The present invention relates to a set of two-dimentional preparative chromatography instrument system with on-line preconcentration function.
Background technology
High activity chemical composition in natural drug is one of important sources of new drug, along with deepening continuously of research, the separated acquisition of a large amount of high-load composition, researcher turns to the separation of microchemistry composition in natural drug gradually, finds new component wherein.Compared with high-load composition, the micro constitutent in natural drug is more easily subject to other composition disturbing effects in detachment process, separating monitoring difficulty, and conventional separation techniques uses raw material dosage large, and separation efficiency is low, therefore needs efficient separating tool.
Preparative chromatography has powerful separating power, is the main tool that natural drug is separated.Natural products composition is complicated, and single chromatographic resolution limited efficiency, needs through separating for several times, uses different chromatographic resolution pattern just can reach and be satisfied with separating effect in detachment process.Except considering the complementarity of different chromatogram mode, preparative chromatography also will consider preparative-scale problem in detachment process, needs overload loading to ensure to prepare flux.Online Two way chromatograms by the isolated sample of the first dimension preparative chromatography directly or after special excuse collection, enter the second dimension preparative chromatography be separated, can simplify detachment process, increase work efficiency.Shao Ping (Chinese patent, CN101791491A) the two-dimentional preparing chromatography system that a set of online basic, normal, high pressure combines is devised, by six-way valve and software, two preparing chromatography systems are coupled together, during first dimension preparative chromatography is separated, sample overload loading is run, intercepting target flow point enters the second dimension preparative chromatography and is separated further, for solving the contradiction between overload sample introduction and separating power, improve chromatogram separating capacity.Zhang Weibing devises a kind of Quasi dynamic two dimension preparing chromatography system and separating substances method (Chinese patent, CN102914610A, CN202870047U), by T-valve, two preparative chromatography posts are connected, by Vavle switching, the component that the first dimension preparative chromatography post is separated is transferred to the second dimension preparative chromatography post to be separated, equally for solving the contradiction between overload sample introduction and separating power.Above system only has simple flow point forwarding function, large volume flow point containing target component directly enters the second dimension preparing chromatography system can have a strong impact on its separating power, above system does not have enrichment function simultaneously, raising first is needed to tie up preparative chromatography applied sample amount to ensure and prepare flux, and micro constitutent is under heavy overload ruuning situation, be difficult to be separated and monitoring, affect separating effect.
Summary of the invention
The present invention relates to a set of two-dimentional preparative chromatography instrument system with on-line preconcentration function.Native system is by chromatogram flow channel switching valve (two ten-way valves, two six-way valves or banked direction control valves), and chromatographic column (preparative column, guard column and trapping column), solvent pump (comprising mobile phase pump and mobile phase adjustment pump) and detecting device form.It is characterized in that passing through Vavle switching, mobile phase regulates, and the mode that trapping column three combines, achieve the interface function of cyclical chromatography interface and Two way chromatograms, thus complete two peacekeeping multi-dimensional chromatographs and be separated, the separating effect of simultaneity factor can not increase with loading volume and the carrying out and decline of detachment process.In addition, native system also possesses the concentration and recovery function to be separated final products, thus simplifies sample drying process, and is conducive to the sex change of avoiding sample in heat drying process.
There is the two-dimentional preparing chromatography system of on-line preconcentration function, comprise a mobile phase pump, three three-way cut-off valves, two ten-way valves, a quantitative loop, a guard column, a trapping column, an adjustment pump, two two six-way valves, threeway, chromatographic detector, the first dimension preparative column a, the second dimension preparative column b and other associated lines composition;
Wherein two six-way valve b, the first dimension preparative column a and second dimension preparative column b form post selective system;
Above-mentioned each parts order of connection is as described below: two ten-way valve interfaces 1. successively with three-way cut-off valve a, prepare pump and prepare pump mobile phase and be connected, the 3rd the interface emptying outlet of three-way cut-off valve a; 3. 2. two ten-way valve interfaces be connected with interface; 1. 4. two ten-way valve interfaces be connected with the interface of two six-way valve I; 2. two ten-way valve interfaces 5. successively through being connected with two six-way valve II interfaces by three-way cut-off valve b, and the 3rd interface of three-way cut-off valve b is emptying outlet; 6. two ten-way valve interfaces are connected with guard column column cap interface; 7. with 10. two ten-way valve interfaces are connected by quantitative loop; 8. two ten-way valve interfaces are sample injection port, and interface is emptying 9.;
1. two six-way valve II interfaces are connected with the post tail interface of guard column; 2. two six-way valve II interfaces are connected with ten-way valve by three-way cut-off valve b; 3. the interface of two six-way valve II is connected with the post tail interface of trapping column; 4. the interface of two six-way valve II is connected with the entrance of chromatographic detector; 4. 5. the interface of two six-way valve II be connected with the interface of two six-way valve I; 6. the interface of two six-way valve II is connected with the column cap interface of trapping column by threeway, the other end of threeway successively with three-way cut-off valve c, regulate pump and regulate solution and be connected, the 3rd interface of three-way cut-off valve is emptying outlet;
4. 1. two six-way valve PCI interface be connected with two ten-way valve interfaces; 3. 2. two six-way valve PCI interface be connected with the second import and export tieing up preparative column b respectively with interface; 5. 4. two six-way valve PCI interface be connected with the interface of two six-way valve II; 5. 4. two six-way valve PCI interface be connected with the first import and export tieing up preparative column a respectively with interface.
Two-dimensional liquid chromatography sample transfer interface is a trapping column with reservation enrichment function, regulates and makes target component adsorbing and trapping or wash-out transfer by the mobile phase eluting power of trapping column.
Single trapping column can be replaced by many trapping column system.
The post selective system connecting two preparative columns in system can be replaced by multicolumn selective system.
By using many trapping column system and multicolumn selective system, enrichment can be carried out to multiple target component, and carry out the chromatographic resolution preparation of multidimensional respectively.
Native system specifically uses step as follows:
1) loading
After sample solution injects sample amounts ring, adopt the first dimension preparative chromatography mobile phase that sample is imported trapping column after guard column, simultaneously to trapping column input regulator solution, reduce mobile phase eluotropic strength, sample is retained in trapping column to be separated;
2) one dimension is separated
Close mobile phase and regulate pump, application first dimension preparative chromatography mobile phase, sample elution to the first dimension preparative column in trapping column will be retained in and be separated;
3) target component trapping
By Vavle switching, the target component after the first dimension preparative column is separated is transferred to trapping column, simultaneously to trapping column input regulator solution, reduces and regulate strength of mobile phase, make target peak be enriched in trapping column;
4) two dimensional separation
By Vavle switching, the second dimension preparative column is connected in flow path system, adopts the second dimension preparative chromatography mobile phase will be enriched in sample elution to the second in trapping column and tie up preparative column, realize being separated further;
5) sample reclaims
Through the subject component that the second dimension preparative column is separated, namely separation case can collect according to detecting device, also subject component can be trapped again in trapping column, regulate pump input eluting power strong, and the mobile phase of high volatility, target component is dissolved in small size mobile phase, is convenient to recovery sample.
Described 1) loading and 3) in target component trapping process, regulator solution is the weak eluotropic strength solvent dissolved each other with mobile phase; In sample removal process, regulator solution selects eluotropic strength large and the solvent that volatility is high.
Described regulator solution is be conducive to strengthening the solvent that retains in trapping column of sample, comprises the large and solvent that volatility is high of methyl alcohol, acetonitrile, acetone, ethanol or other eluotropic strengths.
Repeat step (2) ~ (3), the effect be separated with dimension chromatographic cycles can be reached; Repeatedly repeat (1) ~ (3) processes, repeatedly can carry out Two way chromatograms separation again after enrich target composition.
The present invention is adopted to have the following advantages compared with classic method:
1) this instrument system can carry out two dimensional separation, in the first dimension preparative chromatography detachment process, by carrying out repeatedly loading and trapping, target component is enriched in trapping column, the applied sample amount of two dimension preparation can be improved, remove the non-targeted composition trapped simultaneously, reduce the interference of impurity to target component in the second dimension chromatographic separation process.Trapping column interface effectively retains enriched sample and one dimension separation component, effectively avoids sample volume to transship and solvent effect problem, and the loss of post effect is little, ensures two dimensional separation effect.
2) this instrument system easily extensible carries out repeatedly multi-cycle separation and is separated with multidimensional, and separating effect can not increase with being separated number of times increase with sample volume and decline.
3) this instrument system also possesses the concentration and recovery function to be separated final products, thus simplifies sample drying process, is conducive to the sex change avoiding sample in heat drying process.
Accompanying drawing explanation
Fig. 1 is two-dimentional preparing chromatography system structural drawing;
Fig. 2 is many trapping column system construction drawing;
Fig. 3 is multicolumn selective system structural drawing;
Fig. 4 is Two way chromatograms system cloud gray model schematic diagram.
Wherein, 1-mobile phase pump; 2-three-way cut-off valve a; 3-two ten-way valves; 4-three-way cut-off valve b; 5-post selective system; 6-quantitative loop; 7-guard column; 8-trapping column; 9-regulates pump; 10-two six-way valve I; 11-three-way cut-off valve c; 12-threeway; 13-six-way valve II; 14-chromatographic detector; 15-many trapping column system; 16-multicolumn selective system; A-first ties up preparative column; B-second ties up preparative column.
Fig. 1 is the two-dimentional preparing chromatography system be made up of two ten-way valves and two six-way valves; Fig. 2 to be replaced in Fig. 1 10, Fig. 3 to replace in Fig. 1 12 can form can the preparing chromatography system that is separated of multidimensional.
Embodiment
Now be described in further details the present invention with accompanying drawing, embodiment is only limitted to the present invention is described in conjunction with the embodiments, but not limitation of the invention.
Embodiment 1 single loading is prepared for the two dimension of 40% content composition
This experiment plan prepares 40% content composition in natural plant extracts.First dimension preparative chromatography post and trapping column are 10um Chromatorex C18 filler preparative chromatography post, second dimension preparative chromatography post is 5um Microsorb C18 filler preparative chromatography post, first dimension preparative chromatography mobile phase is 60% methyl alcohol, and the second dimension preparative chromatography mobile phase is 45% acetonitrile.Sample solution in quantitative loop, enters trapping column after ten-way valve and guard column, inputs water simultaneously and reduces mobile phase eluting power, target component is retained in trapping column.Adopt the first dimension preparative chromatography mobile phase wash-out trapping column, sample is brought into the first dimension preparative chromatography post and be separated.By the flow point containing target component by Vavle switching, be transferred in trapping column, input water liquid simultaneously and reduce mobile phase eluting power, target component is retained in trapping column.Change mobile phase, by Vavle switching, by the second dimension preparative chromatography mobile phase wash-out trapping column, the target component sample elution to the second of enrichment dimension preparative chromatography post is separated.Target component is enriched in trapping column by the mode regulated with mobile phase again, and by regulating pump by the product-collecting after purifying in small size methyl alcohol, after testing, product purity can reach 98%.
Embodiment more than 2 loading is prepared for the two dimension of 0.2% content composition
This experiment plan prepares 0.2% content composition in natural plant extracts.First dimension preparative chromatography post is 10um Chromatorex C18 filler preparative chromatography post, trapping column is 10um Calesil C18 filler chromatographic column, second dimension preparative chromatography post is 5um Microsorb C18 filler preparative chromatography post, first dimension preparative chromatography mobile phase is 80% methyl alcohol, and the second dimension preparative chromatography mobile phase is 75% methyl alcohol.Sample solution in quantitative loop, enters trapping column after ten-way valve and guard column, inputs water simultaneously and reduces mobile phase eluting power, target component is retained in trapping column.Adopt the first dimension preparative chromatography mobile phase wash-out trapping column, sample elution to the first is tieed up preparative chromatography post and is separated.By the flow point containing target component by Vavle switching, be transferred in trapping column, input regulator solution simultaneously and reduce mobile phase eluting power, target component is retained in trapping column.Repeat loading, one dimension is separated and the process of on-line preconcentration, be enriched in accumulative for target component in trapping column.Change mobile phase, make the second dimension preparative chromatography mobile phase flow through trapping column by Vavle switching, the target component sample elution to the second of enrichment dimension preparative chromatography post is separated.Target component is enriched in trapping column by the mode regulated with mobile phase again, by regulating pump by the product-collecting after purifying in small size methyl alcohol.After testing, product purity can reach 98%.
Claims (9)
1. there is the two-dimentional preparing chromatography system of on-line preconcentration function, it is characterized in that: comprise a mobile phase pump (1), three three-way cut-off valves (2,4,11), one two ten-way valves (3), a quantitative loop (6), a guard column (7), a trapping column (8), an adjustment pump (9), two two six-way valves (10,13), threeway (12), chromatographic detector (14), the first dimension preparative column a, the second dimension preparative column b and other associated lines composition;
Wherein two six-way valve I(10), the first dimension preparative column a and second dimension preparative column b forms post selective system (5);
Above-mentioned each parts order of connection is as described below: two ten-way valve (3) interfaces 1. successively with three-way cut-off valve a(2), prepare pump (1) and prepare pump mobile phase (1-A with 1-B) and be connected, three-way cut-off valve a(2) the 3rd interface emptying outlet; 3. 2. two ten-way valve (3) interfaces be connected with interface; Two ten-way valve (3) interfaces 4. with two six-way valve I(10) interface be 1. connected; 5. two ten-way valve (3) interfaces pass through successively by three-way cut-off valve b(4) with two six-way valve II(13) 2. interface be connected, three-way cut-off valve b(4) and the 3rd interface be emptying outlet; 6. two ten-way valve (3) interfaces are connected with guard column (7) column cap interface; 7. with 10. two ten-way valve (3) interfaces are connected by quantitative loop (6); 8. two ten-way valve (3) interfaces are sample injection port, and interface is emptying 9.;
Two six-way valve II(13) 1. interface be connected with the post tail interface of guard column (7); Two six-way valve II(13) interface is 2. by three-way cut-off valve b(4) be connected with ten-way valve (3); 3. the interface of two six-way valve II is connected with the post tail interface of trapping column; Two six-way valve II(13) interface be 4. connected with the entrance of chromatographic detector (14); Two six-way valve II(13) interface 5. with two six-way valve I(10) interface be 4. connected; Two six-way valve II(13) interface be 6. connected with the column cap interface of trapping column (8) by threeway (12); the other end of threeway (12) successively with three-way cut-off valve c(11), regulate pump (9) and regulate solution (9-A with 9-B) and be connected, three-way cut-off valve c(11) the 3rd interface be emptying outlet;
Two six-way valve I(10) 4. 1. interface be connected with two ten-way valve (3) interfaces; Two six-way valve I(10) 3. 2. interface be connected with the second import and export tieing up preparative column b respectively with interface; Two six-way valve I(10) interface 4. with two six-way valve II(13) interface be 5. connected; Two six-way valve I(10) 5. 4. interface be connected with the first import and export tieing up preparative column a respectively with interface.
2. the two-dimentional preparing chromatography system with on-line preconcentration function according to claim 1, it is characterized in that: two-dimensional liquid chromatography sample transfer interface is a trapping column (8) with reservation enrichment function, regulate and make target component adsorbing and trapping or wash-out transfer by the mobile phase eluting power of trapping column.
3. the two-dimentional preparing chromatography system with on-line preconcentration function according to claim 1, is characterized in that: single trapping column (8) can be replaced by many trapping column system (15).
4. the two-dimentional preparing chromatography system with on-line preconcentration function according to claim 1, is characterized in that: the post selective system (5) connecting two preparative columns in system can be replaced by multicolumn selective system (16).
5. any one according to claim 1 or 3 or 4 has the two-dimentional preparing chromatography system of on-line preconcentration function, it is characterized in that: by the many trapping column system described in use claim 3 or 4 and multicolumn selective system, enrichment can be carried out to multiple target component, and carry out the chromatographic resolution preparation of multidimensional respectively.
6. there is an application for the two-dimentional preparing chromatography system of on-line preconcentration function as claimed in claim 1, it is characterized in that: native system specifically uses step as follows:
1) loading
After sample solution injects sample amounts ring (6), adopt the first dimension preparative chromatography mobile phase that sample is imported trapping column (8) after guard column (7), simultaneously to trapping column (8) input regulator solution, reduce mobile phase eluotropic strength, sample is retained in trapping column to be separated;
2) one dimension is separated
Closedown mobile phase regulates pump (9), and application first dimension preparative chromatography mobile phase, will be retained in sample elution to the first dimension preparative column (a) in trapping column (8) and be separated;
3) target component trapping
By Vavle switching, the target component after the first dimension preparative column (a) is separated is transferred to trapping column (8), simultaneously to trapping column (8) input regulator solution, reduces and regulate strength of mobile phase, make target peak be enriched in trapping column;
4) two dimensional separation
By Vavle switching, the second dimension preparative column (b) is connected in flow path system, adopts the second dimension preparative chromatography mobile phase will be enriched in sample elution to the second in trapping column and tie up preparative column (b), realize being separated further;
5) sample reclaims
Through the subject component that the second dimension preparative column (b) is separated, namely separation case can collect according to detecting device, also subject component can be trapped again in trapping column (8), regulate pump input eluting power strong, and the mobile phase of high volatility, target component is dissolved in small size mobile phase, is convenient to recovery sample.
7. application according to claim 6, is characterized in that:
Described 1) loading and 3) in target component trapping process, regulator solution is the weak eluotropic strength solvent dissolved each other with mobile phase; In sample removal process, regulator solution selects eluotropic strength large and the solvent that volatility is high.
8. application according to claim 7, is characterized in that:
Described regulator solution is be conducive to strengthening the solvent that retains in trapping column of sample, comprises the large and solvent that volatility is high of methyl alcohol, acetonitrile, acetone, ethanol or other eluotropic strengths.
9. application according to claim 6, is characterized in that:
Repeat step (2) ~ (3) in claim 6, the effect be separated with dimension chromatographic cycles can be reached; Repeatedly repeat (1) ~ (3) process in claim 6, repeatedly can carry out Two way chromatograms separation again after enrich target composition.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002082071A1 (en) * | 2001-04-05 | 2002-10-17 | The President And Fellows Of Harvard College | Automated capillary liquid chromatography small volume analysis system |
| EP1455185A1 (en) * | 2003-03-06 | 2004-09-08 | Hitachi High-Technologies Corporation | Liquid chromatograph mass spectrometer |
| JP2005214897A (en) * | 2004-01-30 | 2005-08-11 | Shimadzu Corp | Liquid chromatograph |
| CN1785476A (en) * | 2004-12-10 | 2006-06-14 | 清华大学 | Full bidimensional capillary liquid chromatography separation system |
| CN101169392A (en) * | 2006-10-25 | 2008-04-30 | 中国科学院大连化学物理研究所 | Two-dimensional highly effective liquid phase chromatographic device and its uses |
| CN102961892A (en) * | 2011-09-01 | 2013-03-13 | 李贺然 | Preparative multidimensional liquid chromatographic instrument |
-
2013
- 2013-12-13 CN CN201310691030.7A patent/CN104713973B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002082071A1 (en) * | 2001-04-05 | 2002-10-17 | The President And Fellows Of Harvard College | Automated capillary liquid chromatography small volume analysis system |
| EP1455185A1 (en) * | 2003-03-06 | 2004-09-08 | Hitachi High-Technologies Corporation | Liquid chromatograph mass spectrometer |
| JP2005214897A (en) * | 2004-01-30 | 2005-08-11 | Shimadzu Corp | Liquid chromatograph |
| CN1785476A (en) * | 2004-12-10 | 2006-06-14 | 清华大学 | Full bidimensional capillary liquid chromatography separation system |
| CN101169392A (en) * | 2006-10-25 | 2008-04-30 | 中国科学院大连化学物理研究所 | Two-dimensional highly effective liquid phase chromatographic device and its uses |
| CN102961892A (en) * | 2011-09-01 | 2013-03-13 | 李贺然 | Preparative multidimensional liquid chromatographic instrument |
Cited By (27)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106645506B (en) * | 2015-08-20 | 2019-04-09 | 中国科学院大连化学物理研究所 | A kind of three-dimensional liquid chromatographic separation system |
| CN106645506A (en) * | 2015-08-20 | 2017-05-10 | 中国科学院大连化学物理研究所 | Three-dimensional liquid chromatogram separation system |
| CN105938130B (en) * | 2016-06-30 | 2018-04-20 | 朱靖博 | It is a kind of to integrate separation method exploitation, the natural drug two dimension preparative chromatograph of on-line preconcentration and its method of work |
| CN105938130A (en) * | 2016-06-30 | 2016-09-14 | 朱靖博 | Natural drug two-dimensional preparation chromatographic instrument with integrated functions of separation method development and online separation-enrichment and work method thereof |
| WO2018188184A1 (en) * | 2017-04-12 | 2018-10-18 | 岛津企业管理（中国）有限公司 | Multifunctional on-line combination device for temperature and pressue increase-assisted extraction, trapping, and chromatographic separation |
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