US2008053908A1PendingUtilityA1

High pressure flash chromatography

49
Assignee: CHORDIA LALITPriority: Sep 1, 2006Filed: Sep 4, 2007Published: Mar 6, 2008
Est. expirySep 1, 2026(~0.1 yrs left)· nominal 20-yr term from priority
Inventors:Lalit ChordiaHarbaksh SidhuTodd PalcicJohn Christopher Whelan
G01N 30/34B01D 15/165B01D 15/20
49
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Claims

Abstract

A method for separating a sample using high pressure flash chromatography is provided. The method comprises the steps of: i) providing a pressurized vessel containing an adsorption material; ii) pressurizing a compressible fluid, optionally containing a cosolvent, to create a mobile phase; iii) premixing the sample with the mobile phase or optionally placing the sample in the pressurized vessel; iv) eluting the mobile phase through the pressurized vessel, to obtain a separated sample; v) heating the mobile phase containing the separated sample after the mobile phase exits the pressurized vessel to remove the compressible fluid; and iv) collecting the separated sample. The pressurized vessel contains an adsorption material having a particle size of 10-100 microns, and the pressure of the adsorption vessel is held at 50-350 bar during elution. Also provided is an apparatus for carrying out the above method.

Claims

exact text as granted — not AI-modified
1 . A high pressure flash chromatography apparatus comprising:
 a) a pressurized vessel containing an adsorption material having a particle size of 10-100 microns;   b) a pumping means for pressurizing and delivering a mobile phase to the pressurized vessel, the mobile phase comprising a compressible fluid;   c) a loading means for loading a sample into the pressurized vessel and onto the adsorption material;   d) a pressure controlling means for controlling the pressure of the mobile phase exiting the pressurized vessel;   e) a heat exchanger for controlling the temperature of the mobile phase exiting said pressure controlling means;   f) a collection means for collecting fractions of the sample; and   g) a means for directing the mobile phase exiting the heat exchanger to the collection means.   
     
     
         2 . The apparatus of  claim 1 , further comprising a second pumping means to deliver a cosolvent to the pressurized vessel. 
     
     
         3 . The apparatus of  claim 2 , wherein the mobile phase delivered to the pressurized vessel is between 10° C. and 150° C. 
     
     
         4 . The apparatus of  claim 2 , further comprising means for controlling the flow of the cosolvent to the pressurized vessel. 
     
     
         5 . The apparatus of  claim 2 , further comprising a pumping means after the pressurized vessel and before the collection means. 
     
     
         6 . The apparatus of  claim 2 , further including a detection means for detecting for detecting compound(s) of interest in the sample. 
     
     
         7 . The apparatus of  claim 2 , wherein the adsorption material is dry packed in the pressurized vessel 
     
     
         8 . The apparatus of  claim 2 , wherein said adsorption material is piston packed. 
     
     
         9 . The apparatus of  claim 2 , wherein the pressurized vessel contains a separate cartridge containing the adsorption material. 
     
     
         10 . The apparatus of  claim 2 , wherein the adsorption material is a silica-based material. 
     
     
         11 . The apparatus of  claim 10 , wherein the silica-based material has a particle size of between about 20 to about 70 microns 
     
     
         12 . The apparatus of  claim 2 , wherein the mobile phase further comprises a cosolvent. 
     
     
         13 . The apparatus of  claim 2 , wherein said collection means is selected from the group consisting of one or more fraction collectors, cyclonic separators, trapping devices, solid phase cartridges, cryofocusing systems and any combination of these. 
     
     
         14 . The apparatus of  claim 2 , wherein said loading means is an injection valve. 
     
     
         15 . The apparatus of  claim 2 , wherein the loading means is an injection pump in combination with an injection valve. 
     
     
         16 . The apparatus of  claim 2 , wherein the loading means is manually pouring the sample into the pressurized vessel. 
     
     
         17 . The apparatus of  claim 1  or  2  further comprising one or more frits in the pressurized vessel. 
     
     
         18 . The apparatus of  claim 1  or  7 , wherein said loading means is a loading cavity in the pressurized vessel or optionally in the cartridge. 
     
     
         19 . The apparatus of  claim 2  further comprising a recycling system placed after said collection means to recycle the compressible fluid. 
     
     
         20 . A method for separating a sample using high pressure flash chromatography, the method comprising the steps of:
 i) providing a pressurized vessel containing an adsorption material;   ii) pressurizing a compressible fluid, optionally containing a cosolvent, to create a mobile phase;   iii) eluting the mobile phase and the sample through the pressurized vessel, to obtain a separated sample;   iv) heating the mobile phase containing the separated sample after the mobile phase exits the pressurized vessel to facilitate the separation of the compressible fluid; and   v) collecting the separated sample,
 wherein the pressurized vessel contains an adsorption material having a particle size of 10-100 microns, and 
 the pressure of the adsorption vessel is held at 50-350 bar during elution. 
   
     
     
         21 . The method of  claim 20 , wherein the mobile phase is heated before entering the pressurized vessel. 
     
     
         22 . The method of  claim 20 , wherein the adsorption material is dry packed into the pressurized vessel. 
     
     
         23 . The method of  claim 20 , wherein the adsorption material is piston packed into the pressurized vessel. 
     
     
         24 . The method of  claim 20 , wherein the adsorption material is present in a cartridge within the pressurized vessel. 
     
     
         25 . The method of  claim 20 , wherein the sample is loaded directly onto the cartridge within the pressurized vessel. 
     
     
         26 . The method of  claim 20 , wherein the sample is premixed with the mobile phase prior to elution through the pressurized vessel. 
     
     
         27 . The method of  claim 20 , wherein the mobile phase is recycled after collecting the separated sample. 
     
     
         28 . The method of  claim 20 , wherein the compressible fluid is carbon dioxide. 
     
     
         29 . The method of  claim 20 , wherein the cosolvent is an organic solvent. 
     
     
         30 . The method of  claim 20 , wherein said adsorption material is a silica-based material. 
     
     
         31 . The method of  claim 20 , wherein the mobile phase comprises a compressible fluid and a cosolvent. 
     
     
         32 . The method of  claim 20 , wherein the sample is loaded into the cosolvent prior to being mixed with the compressible fluid.

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