CN2469454Y - Closed continuous column chromatography analyse device - Google Patents
Closed continuous column chromatography analyse device Download PDFInfo
- Publication number
- CN2469454Y CN2469454Y CN 01212710 CN01212710U CN2469454Y CN 2469454 Y CN2469454 Y CN 2469454Y CN 01212710 CN01212710 CN 01212710 CN 01212710 U CN01212710 U CN 01212710U CN 2469454 Y CN2469454 Y CN 2469454Y
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- China
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- chromatography
- eluent
- condensing tube
- column
- reflux condensing
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Abstract
The utility model relates to a sealing continuous column chromatography device and consists of a temperature control magnetic stirring apparatus, a round bottom matrass, a chromatography column, an eluate steam through pipe, a discharge pipe with a piston, a jet flow vacuum pump, and a circulating water flume. When the utility model is used, the eluate is in a basically close recycling state and enables the chromatography operation keeping an anoxic condition, the chromatography parameter stably, the separation efficiency high, and the eluent volatility losing slightly. And the utility model is favorable for protecting the separated material, increasing the quantity, enhancing the quality, reducing the environmental pollution, and improving the working conditions. The production period of the device is short, the dosage of the eluent amount is little, and the labor intensity is low.
Description
The utility model relates to a kind of complex component that is used for and separates the column chromatography device of purifying.
Column chromatography is that complex component separates the very effective means of purifying, and is usually used in the extraction and the purifying of biochemical product and natural drug effective constituent.Existing column chromatography equipment includes chromatographic column, separate often a time-consuming very long process, and labour intensity is big, diffuse to aerial in the eluent after the volatile toxic organic compound volatilization, not only cause the waste of eluent, and pollute, it is healthy to influence the workman.In addition, eluent with also can absorb airborne moisture during air contacts, water cut is increased gradually, these moisture can be used as the silica gel adsorption of chromatographic column, change the water cut of silica gel, influence the separation efficiency of chromatographic column.
The purpose of this utility model is at above-mentioned present situation, and it is little to aim to provide a kind of eluent volatilization loss, helps environmental protection, the continuous column chromatography device of the sealing that the eluant, eluent consumption is few, separation efficiency is high.
The implementation of the utility model purpose is, seals continuous column chromatography device, includes chromatographic column 7.Round bottom cucurbit 2 places temperature control magnetic stirring apparatus 1, and chromatographic column is made of chromatography main column 7, eluent steam siphunculus 13, drain pipe 3.The eluent steam channel is connected on chromatography main column upper and lower position.Drain pipe exports down with the chromatography main column and communicates, and bilateral piston 4,6, thief hole 5 are arranged on the pipe.Chromatographic column upper and lower respectively with reflux condensing tube 8, the airtight connection of round bottom cucurbit 2 grounds.Reflux condensing tube has condensate water import and export 12,9, suitable for readingly communicates with jet vacuum pump 15, and jet vacuum pump connects circulating water chennel 16, water pump 18.Circulating water chennel has freeing port 17 and water inlet, and water inlet communicates with the condensation-water drain 9 of reflux condensing tube.Reflux condensing tube by joint 10, take over 11 and link to each other with jet vacuum pump 15.
Accompanying drawing is the utility model structural representation.
With reference to accompanying drawing, well heater adopts temperature control magnetic stirring apparatus 1, and interior dress whiteruss is temperature automatically controlled by electric contact thermometer.Round bottom cucurbit 2 is three mouthfuls of cucurbits, the eluent that interior Sheng prepares, and the bottom is immersed in the paraffin, and middle port links to each other with the chromatographic column break-in, and left side mouth is a charging aperture, right mouthful plug in thermometer.
Chromatography main column 7 adopts dry method or wet method to pack into.Layer of silica gel top dress is mixed with the silica gel of an amount of sample to be separated, spreads one deck absorbent cotton topmost.Notice that material to be separated should be a little less than the outlet of steam channel 13.
During the work of this device, heating of temperature control magnetic stirring apparatus and rotation magnet rotor stir the eluent in the round bottom cucurbit, make generation steam.Steam rises along steam channel 13, and by the condensate water condensation that goes out from water inlet 12 entery and delivery ports 9, condensed fluid splashes into silica gel column chromatography 7 after drain pipe 3 splashes in the round bottom cucurbit in reflux condensing tube 8, realizes continuous chromatography.Drain pipe has three effects: one, splash into speed by bilateral piston 4,6 control condensed fluids, i.e. chromatography speed; Two, closure piston 4,6, and the stick harness in the rotation thief hole 5 makes the hole of sampling hole wall communicate with plunger hole, extracts stick harness, can take a sample and detect, to realize the monitoring to separating effect; Three, under the situation that does not change the system negative pressure, can in the round bottom cucurbit, replenish eluent by thief hole.
Done the separation purification test of semi-synthetic-HCPT with common column chromatography and this device:
Sample is: the semi-synthetic potpourri of 10-HCPT that contains complicated ingredients such as 10-HCPT, camptothecine, deoxycamptothecine, 10-Methoxycamptothecine, 11-methoxycamptothecine and other impurity.Eluent adopts methenyl choloride to add an amount of methyl alcohol.Make column chromatography with silica gel, chromatographic column diameter 50mm, high 900mm, the silica gel of interior dress, dress sample 15g through suitably activating.
Common column chromatography: adopt gradient elution, the about 3ml/ branch of chromatography speed separates when finishing consuming eluent 27500ml altogether, lasts 152 hours, reclaims eluent 19663ml, volatilization loss 7837ml during vacuum distillation.Product purity 92.4%.
This device: enter the hydraulic pressure of jet vacuum pump by control, make eluent, and keep the silica gel sky to have unnecessary liquid to cover the steam channel outlet all the time flowing into the round bottom cucurbit 50 ℃ of boilings.The about 3ml/ branch of chromatography speed lasts 126 hours, and eluant, eluent consumes 2300ml altogether, and behind impurity screening and the product, negative pressure reclaims 1950ml, volatilization loss 350ml.Product purity 96.6%.
From above-mentioned experiment as seen, few with this device eluent volatilization loss, consumption is little, and the separation efficiency height separates the product purity height after purifying
The utility model eluent is in the recycling state of base closed; keep anoxia condition when making chromatography; chromatography parameter stability, separation efficiency height, eluent volatilization loss are little, help protecting the unsettled separated material of high activity, help reducing environmental pollution, improve working environment.This device has shortened the production cycle with wash-out and the combination of product condensing crystallizing two procedures, has reduced the eluant, eluent consumption, has reduced labour intensity.
Claims (2)
1, seal continuous column chromatography device, include chromatographic column, it is characterized in that round bottom cucurbit (2) places temperature control magnetic stirring apparatus (1), chromatographic column is by chromatography main column (7), eluent steam siphunculus (13), drain pipe (3) constitutes, the eluent steam channel is connected on the chromatography main column, upper/lower positions, drain pipe exports down with the chromatography main column and communicates, bilateral piston (4) is arranged on the pipe, (6), thief hole (5), on the chromatographic column, down respectively with reflux condensing tube (8), the airtight connection of round bottom cucurbit (2) ground, reflux condensing tube has condensate water to advance, outlet (12), (9), reflux condensing tube is suitable for reading to communicate with jet vacuum pump (15), jet vacuum pump connects circulating water chennel (16), water pump (18), circulating water chennel has freeing port (17) and water inlet, and water inlet communicates with the condensation-water drain (9) of reflux condensing tube.
2,, it is characterized in that reflux condensing tube passes through joint (10), adapter (11) links to each other with jet vacuum pump (15) according to claims 1 described device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01212710 CN2469454Y (en) | 2001-03-12 | 2001-03-12 | Closed continuous column chromatography analyse device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01212710 CN2469454Y (en) | 2001-03-12 | 2001-03-12 | Closed continuous column chromatography analyse device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN2469454Y true CN2469454Y (en) | 2002-01-02 |
Family
ID=33631835
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 01212710 Expired - Fee Related CN2469454Y (en) | 2001-03-12 | 2001-03-12 | Closed continuous column chromatography analyse device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN2469454Y (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102068832A (en) * | 2010-11-23 | 2011-05-25 | 孙俊 | Normal pressure column chromatography device under closed environment |
| CN101954202B (en) * | 2009-07-16 | 2012-07-25 | 中国科学院化学研究所 | Constant-pressure closed ascending chromatographic column device and application method thereof |
| CN104028006A (en) * | 2014-06-26 | 2014-09-10 | 湖南师范大学 | Chromatographic device |
| CN104941250B (en) * | 2015-05-27 | 2016-10-26 | 湖南师范大学 | Chromatographic apparatus |
-
2001
- 2001-03-12 CN CN 01212710 patent/CN2469454Y/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101954202B (en) * | 2009-07-16 | 2012-07-25 | 中国科学院化学研究所 | Constant-pressure closed ascending chromatographic column device and application method thereof |
| CN102068832A (en) * | 2010-11-23 | 2011-05-25 | 孙俊 | Normal pressure column chromatography device under closed environment |
| CN104028006A (en) * | 2014-06-26 | 2014-09-10 | 湖南师范大学 | Chromatographic device |
| CN104028006B (en) * | 2014-06-26 | 2015-09-16 | 湖南师范大学 | Chromatographic apparatus |
| CN104941250B (en) * | 2015-05-27 | 2016-10-26 | 湖南师范大学 | Chromatographic apparatus |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |