CN100384499C - Fast pneumatic system for preparing columnar chromatograph and its utilization - Google Patents
Fast pneumatic system for preparing columnar chromatograph and its utilization Download PDFInfo
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- CN100384499C CN100384499C CNB2006100144573A CN200610014457A CN100384499C CN 100384499 C CN100384499 C CN 100384499C CN B2006100144573 A CNB2006100144573 A CN B2006100144573A CN 200610014457 A CN200610014457 A CN 200610014457A CN 100384499 C CN100384499 C CN 100384499C
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Abstract
A pneumatic fast column chromatography system is composed of a negative-pressure unit for filling flowing phase and a medium-pressure unit for eluting the flowing phase. Its application method is also disclosed. When a 10-way valve is in the first state, the flowing phase is filled from an open solvent tank into a sealed one under negative pressure while the chromatographic column is eluted by the flowing phase from the second sealed solvent tank via medium-pressure channel. When the flowing phase in the second tank is consumed off, it is switched to the second state, the flowing phase is filled from the open solvent tank into the second sealed one and the chromatographic column is eluted by the first sealed one.
Description
Technical field
The present invention relates to a kind of quick preparative column chromatographic system, particularly a kind of pneumatic quick preparative column chromatographic system and using method thereof.
Background technology
Fast preparative column chromatographic system (Flash Chrimatography) is to be the column chromatography system of foundational development with the dry method column chromatography, is mainly used in combinatorial chemistry, the preparation purifying of the blend sample in synthetic chemistry and the natural product chemistry fast.Existing quick preparative chromatography system can be divided into two big classes according to the type of drive of mobile phase solvent: the air-driven type and the type that surges, respectively with Compressed Gas and liquid phase pump as the solvent driving force.Wherein, the former can't onlinely replenish and the change mobile phase solvent, makes continued operation relatively poor; The latter controls conveniently, the automaticity height, but price is very high.
Fig. 1 is existing pneumatic system flow chart.Mobile phase solvent is contained in the receiver of complete closed in advance, and whole system pressure inside is generally about 75-100psi.Because chromatographic column is a medical disposable material, column jecket adopts polytetrafluoroethylmaterial material more.During operation, chromatographic column is positioned over and is full of (as shown in Figure 3) in the compressed-air actuated pressurized tank, and the pressure balance with inside and outside the assurance post prevents that cylinder from occurring breaking because of hypertonia.Along with constantly carrying out of wash-out, add eluotropic strength mutually mobile or the mobile phase of increase if desired, at first shutdown system bleeds off the compressed air in the system, opens receiver then and replenishes or change the phase that flows.Operating process is very loaded down with trivial details.In order to reduce trouble, existing a lot of products all adopt bigger receiver to avoid supplementing solvent.Increase cost like this, can cause the waste of unnecessary mobile phase solvent simultaneously, and still can't online change mobile phase solvent.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of pneumatic quick preparative column chromatographic system and using method thereof.By technological improvement and unique flow path designs, thereby the canned of mobile phase solvent and wash-out function are integrated effectively, have solved the defective that existing pneumatic system can't continued operation.Like this, whole system has realized continuous operation, and can onlinely replenish the composition that flows mutually and change mobile phase solvent, thereby has broken through the technical bottleneck of existing pneumatic system, has greatly improved the practicality of product.
The purpose of this invention is to provide a kind of pneumatic quick preparative column chromatographic system.
Another object of the present invention provides a kind of using method of pneumatic quick preparative column chromatographic system.
Pneumatic quick preparative column chromatographic system of the present invention, comprise mobile phase solvent jar and chromatographic column, it is characterized in that system is divided into relatively independent negative pressure part and intermediate pressure section, wherein negative pressure partly is used for the canned function of mobile phase solvent, intermediate pressure section is used for the wash-out function of mobile phase, can switch mutually between two parts.
Mutual switching of the present invention is undertaken by ten-way valve.Described ten-way valve is connected with an open solvent tank and two closed solvent tanks, a vavuum pump, a two-port valve respectively by pipeline, a vent valve, vent valve connects with the compressed air inlet, and two-port valve is orderly connected with injector, chromatographic column, detector, fraction collector.
When ten-way valve during at first kind of state, the compressed air inlet links to each other with the second closed solvent tank, chromatographic column successively, baric flow road in the composition; Open solvent tank links to each other with the first closed solvent tank, vavuum pump successively, forms the negative pressure stream; When ten-way valve switched to second kind of state, the compressed air inlet linked to each other with the first closed solvent tank, chromatographic column successively, baric flow road in the composition; Open solvent tank links to each other with the second closed solvent tank, vavuum pump successively, forms the negative pressure stream.
Pneumatic quick preparative column chromatographic system internal pressure of the present invention is 0-250psi, elution speed 0-1500mL/min, and the preparation sample size is mg level～Kg level.Wherein elution speed is relevant with system pressure, chromatographic column and mobile phase solvent, and the preparation sample size is concrete relevant with the chromatographic column size.
Chromatogram column system of the present invention is surrounded by the chuck of a metal or nonmetallic materials at the outer surface of chromatographic column as shown in Figure 4, and with bolt or alternate manner chuck is fixed.Preferably with the bolt crosswise fixed.The chuck material does not have specific (special) requirements, as long as can tolerate certain pressure, approximately 300psi gets final product metal material such as steel, iron, alloy etc., the withstand voltage polythene material of nonmetallic materials such as heavy wall etc.
The using method of pneumatic quick preparative column chromatographic system of the present invention comprises the steps:
(1) beginning, when ten-way valve switched to first kind of state, under the negative pressure that vavuum pump drives, mobile phase solvent carried out canned from open solvent tank to first closed solvent tank, simultaneously, mobile phase solvent from second closed solvent tank by the baric flow road chromatographic column is carried out wash-out;
(2) when flowing in second closed solvent tank exhausts mutually, use ten-way valve to switch stream to the second kind of state, it is canned to second closed solvent tank from open solvent tank that flow communication is crossed the negative pressure stream, by first closed solvent tank chromatographic column carried out wash-out;
(3) after whole separation process finishes, open vent valve, bleed off the compressed air in the system.
Compared with prior art, the present invention has following beneficial effect;
1. the online canned mode of solvent:
System is divided into relatively independent negative pressure part and intermediate pressure section.Wherein, negative pressure partly is used for the canned function of mobile phase solvent, and intermediate pressure section is used for the wash-out function of mobile phase.Because open solvent tank C is open system, can add different solvents at any time, solved at present can't online change the flow significant deficiency of phase of pneumatic system.
2. the raising of continued operation performance:
By the design of ten-way valve, realize the mutual switching between two parts, thereby just canned the and wash-out function of mobile phase solvent is integrated effectively, solved the defective that existing pneumatic system can't continued operation.
3. after whole separation process finishes, still there is unnecessary solvent in the jar mutually, solvent discharge fully just can must be bled off the compressed air in the system if flow.For addressing this problem, the present invention has designed the vent valve device. any moment, stop instrument work as needs, if closes compression air source, and open vent valve A, and can bleed off the compressed air in the system, make system enter idle state.
4. adopt chromatogram column system of the present invention, can prevent that cylinder under high pressure breaking, compare the existing chromatogram column system of Fig. 3, this device is simple, practical, pressure withstanding degree is high, cost is low also can repeatedly use.
5. simple to operate, safe, can carry out gradient elution, continuity of operation is good, can finish the whole separation process of sample continuously;
6. the reappearance height amplifies easily;
Description of drawings
Fig. 1. the quick preparative column chromatographic system of existing air-driven type flow chart
Fig. 2. the quick preparative column chromatographic system of air-driven type of the present invention flow chart
A is first kind of state, and b is second kind of state.
A wherein: vent valve, B: ten-way valve, C: vavuum pump, D: open mobile phase solvent jar
F: first closed mobile phase solvent jar F: second closed mobile phase solvent jar G: two-port valve,
H: injector, I: chromatographic column J: detector K: fraction collector
Fig. 3. existing chromatogram column system artwork
Fig. 4. chromatogram column system artwork of the present invention
Fig. 5. the vertical view of chromatographic column chuck
The specific embodiment
Below in conjunction with drawings and Examples the present invention is elaborated.
Ten-way valve B is connected with an open solvent tank D and two closed solvent tank E and F, vavuum pump C, a two-port valve G respectively by pipeline, a vent valve A, vent valve A connects with the compressed air inlet, and two-port valve G is orderly connected with injector H, chromatographic column I, detector J, fraction collector K.
As ten-way valve B during at first kind of state a, the compressed air inlet links to each other with the second closed solvent tank F, chromatographic column I successively, baric flow road in the composition; Open solvent tank D links to each other with the first closed solvent tank E, vavuum pump C successively, forms the negative pressure stream; When ten-way valve B switched to second kind of state b, the compressed air inlet linked to each other with the first closed solvent tank E, chromatographic column I successively, baric flow road in the composition; Open solvent tank D links to each other with the second closed solvent tank F, vavuum pump C successively, forms the negative pressure stream.
The using method of the pneumatic quick preparative column chromatographic system of present embodiment comprises the steps:
(1) beginning, when ten-way valve B switches to first kind of state a, under the negative pressure that vavuum pump C drives, mobile phase solvent carries out canned from open solvent tank D to first closed solvent tank E, simultaneously, mobile phase solvent from second closed solvent tank F by the baric flow road chromatographic column I is carried out wash-out;
(2) when flowing among second closed solvent tank F exhausts mutually, use ten-way valve B to switch stream to the second kind of state, it is canned to second closed solvent tank F from open solvent tank D that flow communication is crossed the negative pressure stream, by first closed solvent tank E chromatographic column carried out wash-out;
(3) after whole separation process finishes, open vent valve A, bleed off the compressed air in the system.
Performance test one:
The employing mobile phase solvent is an ethanol-water system, chromatographic column is self-control 35 * 200mm silicagel column (40-60 μ m), and jacket material is the polythene material of pressure withstanding degree 1.6MPa, and pressure source is the nitrogen steel cylinder, outlet pressure 80psi, vacuum means is changed to the Brinkmann vacuum pump.
Testing result is as follows:
(1) system pressure is working properly when 80psi, elution flow rate 300mL/min;
(2) mobile phase can onlinely be replenished and the change solvent, canned speed 1500mL/min;
(3) ten-way valve can carry out two switchings between stream effectively, realizes continual gradient elution;
(4) the instrument ongoing operation is ten minutes, and situation is stable.Eluting solvent 3.1L, about 15 column volumes;
(5) vent valve is working properly.
Performance test two:
The employing mobile phase solvent is an ethanol-water system, and chromatographic column is self-control 47 * 250mm silicagel column (40-60 μ m), and jacket material is a stainless steel, uses air compressor to be source of the gas, outlet pressure 230psi, and vacuum means is changed to the Brinkmann vacuum pump.
Testing result is as follows:
(1) system pressure is working properly when 230psi, elution flow rate 1400mL/min;
(2) mobile phase can onlinely be replenished and the change solvent, canned speed 1500mL/min;
(3) ten-way valve can carry out two switchings between stream effectively, realizes continual gradient elution;
(4) the instrument ongoing operation is ten minutes, and situation is stable.Eluting solvent 6.5L, about 15 column volumes;
(5) vent valve is working properly.
Claims (8)
1. pneumatic quick preparative column chromatographic system, comprise mobile phase solvent jar and chromatographic column, it is characterized in that system is divided into relatively independent negative pressure part and intermediate pressure section, wherein negative pressure partly is used for the canned function of mobile phase solvent, intermediate pressure section is used for the wash-out function of mobile phase, can switch mutually between two parts.
2. quick preparative column chromatographic system as claimed in claim 1 is characterized in that described mutual switching undertaken by ten-way valve.
3. quick preparative column chromatographic system as claimed in claim 2, it is characterized in that described ten-way valve is connected with an open solvent tank and two closed solvent tanks, a vavuum pump, a two-port valve respectively by pipeline, a vent valve, vent valve connects with the compressed air inlet, and two-port valve is orderly connected with injector, chromatographic column, detector, fraction collector.
4. quick preparative column chromatographic system as claimed in claim 3 is characterized in that the compressed air inlet links to each other with the second closed solvent tank, chromatographic column successively, baric flow road in the composition when ten-way valve during at first kind of state; Open solvent tank links to each other with the first closed solvent tank, vavuum pump successively, forms the negative pressure stream; When ten-way valve switched to second kind of state, the compressed air inlet linked to each other with the first closed solvent tank, chromatographic column successively, baric flow road in the composition; Open solvent tank successively with the second closed solvent tank, vavuum pump links to each other, and forms the negative pressure stream.
5. quick preparative column chromatographic system as claimed in claim 1 is characterized in that internal system pressure is 0-250psi, elution speed 0-1500mL/min, and the preparation sample size is mg level～Kg level.
6. as the described quick preparative column chromatographic system of one of claim 1 to 5, it is characterized in that being surrounded by the chuck of a metal or nonmetallic materials at the outer surface of chromatographic column.
7. quick preparative column chromatographic system as claimed in claim 6 is characterized in that described chuck is with the bolt crosswise fixed.
8. as the using method of the described quick preparative column chromatographic system of one of claim 1 to 7, it is characterized in that comprising the steps:
(1) beginning, when ten-way valve switched to first kind of state, under the negative pressure that vavuum pump drives, mobile phase solvent carried out canned from open solvent tank to first closed solvent tank, simultaneously, mobile phase solvent from second closed solvent tank by the baric flow road chromatographic column is carried out wash-out;
(2) when flowing in second closed solvent tank exhausts mutually, use ten-way valve to switch stream to the second kind of state, it is canned to second closed solvent tank from open solvent tank that flow communication is crossed the negative pressure stream, by first closed solvent tank chromatographic column carried out wash-out;
(3) after whole separation process finishes, open vent valve, bleed off the compressed air in the system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100144573A CN100384499C (en) | 2006-06-27 | 2006-06-27 | Fast pneumatic system for preparing columnar chromatograph and its utilization |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100144573A CN100384499C (en) | 2006-06-27 | 2006-06-27 | Fast pneumatic system for preparing columnar chromatograph and its utilization |
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| Publication Number | Publication Date |
|---|---|
| CN1895717A CN1895717A (en) | 2007-01-17 |
| CN100384499C true CN100384499C (en) | 2008-04-30 |
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| CNB2006100144573A Expired - Fee Related CN100384499C (en) | 2006-06-27 | 2006-06-27 | Fast pneumatic system for preparing columnar chromatograph and its utilization |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105388059B (en) * | 2015-10-27 | 2018-06-29 | 仲恺农业工程学院 | A kind of flow injection secondary air separates elution process |
| CN108245931A (en) * | 2016-12-29 | 2018-07-06 | 天津领世生物科技开发有限公司 | Mechanical column chromatography device |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1044339A (en) * | 1988-12-09 | 1990-08-01 | 株式会社日立制作所 | Liquid chromatographic system and its application process |
| CN1317087A (en) * | 1999-07-02 | 2001-10-10 | 奥加诺株式会社 | Chromatographic separatory |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1044339A (en) * | 1988-12-09 | 1990-08-01 | 株式会社日立制作所 | Liquid chromatographic system and its application process |
| CN1317087A (en) * | 1999-07-02 | 2001-10-10 | 奥加诺株式会社 | Chromatographic separatory |
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| CN1895717A (en) | 2007-01-17 |
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Application publication date: 20070117 Assignee: Tianjin Tianda Kaitai Chemical Technology Co., Ltd. Assignor: Aomi Science and Technology Co., Ltd., Tianjin Contract record no.: 2010120000013 Denomination of invention: Fast pneumatic system for preparing columnar chromatograph and its utilization Granted publication date: 20080430 License type: Exclusive License Record date: 20100305 |
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Granted publication date: 20080430 |