IP Library Granted Patent US 8,246,834
Granted Patent B2
US 8,246,834 · App. 13/014,204 · Granted Aug 21, 2012

High pressure flash chromatography

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Quick Facts
Patent No.
US 8,246,834
App. No.
13/014,204
Granted
Aug 21, 2012
Kind
B2
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 (30)

1. A method for separating a sample using high pressure flash chromatography, the method comprising the steps of:

i) providing a pressurized vessel and a cartridge encapsulated therein, wherein the cartridge defines an adsorption material chamber having a diameter between about 1 cm to 20 cm and 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 under high pressure flash chromatography conditions, 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.

2. The method of claim 1 , wherein the mobile phase is heated before entering the pressurized vessel.

3. The method of claim 1 , wherein the sample is loaded directly onto the cartridge within the pressurized vessel.

4. The method of claim 1 , wherein the sample is premixed with the mobile phase prior to elution through the pressurized vessel.

5. The method of claim 1 , wherein the mobile phase is recycled after collecting the separated sample.

6. The method of claim 1 , wherein the compressible fluid is carbon dioxide.

7. The method of claim 1 , wherein the cosolvent is an organic solvent.

8. The method of claim 1 , wherein said adsorption material is a silica-based material.

9. The method of claim 1 , wherein the mobile phase comprises a compressible fluid and a cosolvent.

10. The method of claim 9 , wherein the amount of cosolvent is less than 50 wt % of the mobile phase.

11. The method of claim 9 , wherein the amount of cosolvent is less than 40 wt % of the mobile phase.

12. The method of claim 9 , wherein the amount of cosolvent is less than 30 wt % of the mobile phase.

13. The method of claim 9 , wherein the amount of cosolvent is less than 20 wt % of the mobile phase.

14. The method of claim 9 , wherein the amount of cosolvent is less than 10 wt % of the mobile phase.

15. The method of claim 1 , wherein the sample is loaded into the cosolvent prior to being mixed with the compressible fluid.

16. The method of claim 1 , wherein the cartridge defines an adsorption material chamber having a diameter between about 2 cm to 10 cm.

17. The method of claim 1 , wherein the mobile phase is maintained at a pressure of between about 70 to 150 bar at the top of the pressurized vessel or flash cartridge.

18. The method of claim 1 , wherein the pressure change across the pressurized vessel or flash cartridge from the top to the bottom is between about 1-100 bar.

19. The method of claim 1 , wherein the pressure change across the pressurized vessel or flash cartridge from the top to the bottom is between about 1-20 bar.

20. The method of claim 1 , wherein the pressure change across the pressurized vessel or flash cartridge from the top to the bottom is between about 5-10 bar.

21. The method of claim 1 , wherein the temperature of the pressurized vessel is held at between about 10° C. to 150° C.

22. The method of claim 1 , wherein the temperature of the pressurized vessel is held at between ambient temperature to about 80° C.

23. The method of claim 1 , wherein the particle size is between about 20 to about 70 microns.

24. The method of claim 1 , wherein the particle size is less than about 50 microns.

Assignments (2)
MERGER Recorded Apr 10, 2012
From: THAR INSTRUMENTS INC.
To: WATERS TECHNOLOGIES CORPORATION
Reel/Frame 028021/0088 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 14, 2012
From: CHORDIA, LALIT; SIDHU, HARBAKSH; PALCIC, TODD; WHELAN, JOHN
To: THAR INSTRUMENTS, INC.
Reel/Frame 027699/0714 →