Supercritical-phase mixed chromatography method and installation for implementing same

• US 8,156,788 B2
• Filed: 02/22/2006
• Issued: 04/17/2012
• Est. Priority Date: 02/25/2005
• Status: Active Grant

• Current Assignee: PIC Solution
• Original Assignee: PIC Solution
• Inventors: Shaimi, Mohamed
• Primary Examiner(s): LARKIN, DANIEL SEAN
• Application Number:
  US11/885,023
• Publication Number:
  US 20090049891A1
• Time in Patent Office: 2,246 Days
• Field of Search: 73/233.6, 73/233.7, 73/234.1, 95/82, 95/88, 961/01
• US Class Current: 73/23.36
• CPC Class Codes: B01D 15/1864 using two or more columns
• CPC Class Codes: B01D 15/247 Fraction collectors
• CPC Class Codes: B01D 15/40 using supercritical fluid as mobile phase or eluent
• CPC Class Codes: G01N 2030/326 pumps
• CPC Class Codes: G01N 2030/628 Multiplexing, i.e. several columns sharing a single detector
• CPC Class Codes: G01N 30/02 Column chromatography
• CPC Class Codes: G01N 30/466 with separation columns in parallel

Abstract

A method for the superficial-phase chromatography of a product comprises the steps which are performed continuously in the following order, namely: an operation consisting in pumping a supercritical fluid; and operation consisting of injecting at least one sample of product into at least one chromatography column, a detection operation, and a fraction collection operation. The method comprises at least a first diversion along between an analytical channel and a preparatory channel, which diversion is performed prior to the supercritical fluid pumping operation and the analytical and preparatory channels each including respective supercritical fluid pumping operations. The method is also characterized in that the collection operation is common to both the analytical and preparatory channels. An installation used to implement one such method is described.

Claims

1. A method for the supercritical fluid chromatography of a product, comprising the steps of:

performing a pumping operation for a supercritical fluid,

performing at least one first routing between an analytical path and preparatory path, where the at least one first routing occurs prior to the operation for pumping the supercritical fluid, and where the said analytical and preparatory paths each includes an analytical and preparative column, respectively, and its own supercritical fluid pumping and injection operations, each adjusted according to whether the chromatography is analytical or preparative,

performing an injection operation for at least one sample of the product in one of the analytical or preparative chromatography column,

performing an operation for detection,

performing a regulation of the pressure of the system downstream of the detection,

performing operation for the collection of fractions, and

wherein the regulation of pressure and the collection operation is common to the analytical and preparatory paths.

2. The method according to claim 1, further comprising performing a pumping operation of a modifier in parallel with the pumping operation of the supercritical fluid, and the pumped streams converging to effect the addition of the modifier to the supercritical fluid, toward a main path that is common to the analytical and preparatory paths, upstream of a second routing toward the respective injection operations for the analytical path and the preparatory path.

3. The method according to claim 1, further comprising performing a pumping operation of a modifier, and addition of the modifier to the supercritical fluid taking place upstream of the first routing.

4. The method according to claim 1, wherein the detection operation step is performed by ultraviolet spectroscopy.

5. The method according to claim 1, further comprising performing an operation for controlling the temperature of the supercritical fluid between the pumping operations and the injection operation.

6. The method according to claim 1, wherein the supercritical fluid is carbon dioxide CO₂.

7. An installation for the supercritical fluid chromatography of a product, comprising:

two supercritical fluid pumps, one of analytical capacity, the other of preparative capacity, mounted in parallel, only one of which is operational during operation of the installation,

a first routing valve upstream of said pumps, which is operated so that a supercritical fluid is allowed to flow toward the operational pump,

two systems for the injection of at least one sample of the product into at least two chromatography columns respectively, the injection system and the column size being chosen according to whether the path is for analytical or preparative chromatography, with the systems being mounted in parallel downstream of the pumps and upstream of the columns,

a tubing of narrow diameter to minimize spreading for the chromatographic bands in the analytical path and of wider diameter to minimize the operation pressure drop in the preparative path,

a second routing valve downstream of the columns,

a detection appliance mounted downstream of said second routing valve,

a system for the collection of fractions, and

a back pressure regulator, which is common to the analytical and preparatory paths, and mounted downstream of the detection device but upstream of the system for collection of fractions.

8. The installation according to claim 7, in which a modifier pump equipped with an interchangeable head is placed just upstream of the first routing valve or just upstream of a second routing valve placed downstream of the supercritical fluid pumps.

9. The installation according to claim 8, in which the modifier pump is a low-pressure pump placed upstream of the first routing valve, and in which the supercritical fluid pumps are high-pressure pumps.

10. The installation according to claim 7, further comprising a device for computer control of the different parts of the said installation.

11. The installation according to claim 7, further comprising a heat exchanger placed downstream of the supercritical pumps and upstream of the injection systems.

12. The installation according to claim 7, wherein the supercritical fluid pumps have respective flow capacities with a ratio of at least 2.5.

13. The installation according to claim 7, wherein the detection appliance is an ultraviolet spectrophotometer and includes either two measuring cells mounted in parallel, each after respective chromatography columns, or two interchangeable cells just downstream of a third routing valve placed after the chromatography columns.