Electrochromatographic preconcentration method

• US 5,453,382 A
• Filed: 12/17/1992
• Issued: 09/26/1995
• Est. Priority Date: 08/05/1991
• Status: Expired due to Fees

• Current Assignee: ADVANCED RESEARCH & TECHNOLOGY INSTITUTE
• Original Assignee: Indiana University Foundation (Indiana University)
• Inventors: Soini, Helena A., Novotny, Milos V., Tsuda, Takao
• Primary Examiner(s): Housel, James C.
• Assistant Examiner(s): Pyon, Harold Y.
• Application Number:
  US07/992,232
• Time in Patent Office: 1,013 Days
• Field of Search: 73/23.39, 73/23.42, 204/180.1, 204/182.8, 204/183.3, 204/299 R, 422/69, 422/70, 436/92, 436/98, 436/161, 436/162, 436/178, 436/816, 436/901
• US Class Current: 204/542
• CPC Class Codes: G01N 1/405 by adsorption or absorption
• CPC Class Codes: G01N 2030/027 Liquid chromatography
• CPC Class Codes: G01N 2030/085 using absorbing precolumn
• CPC Class Codes: G01N 2030/285 electrically driven carrier
• CPC Class Codes: G01N 2030/405 re-concentrating or inverting previous separation
• CPC Class Codes: G01N 27/44743 Introducing samples
• CPC Class Codes: G01N 30/08 using an enricher
• CPC Class Codes: Y10T 436/255 including use of a solid sorbent, semipermeable membrane, or liquid extraction

Abstract

Solutions of analytes in concentrations too low for certain analytical techniques such as various capillary electrophoresis techniques are concentrated in a solid-phase adsorption medium by a technique which involves a pressure-gradient-driven adsorption of the analyte followed by a desorption of the analyte and its removal using electroosmotic bulk flow.

Claims

1. A method for treating a source solution containing a suspected analyte to obtain a concentrated solution of said analyte, said method comprising:

(a) passing said source solution through an adsorption medium retained in a column in a first direction by imposing a pressure gradient across said column in the substantial absence of a voltage gradient and under conditions promoting selective immobilization of said analyte by said adsorption medium;

(b) imposing a voltage gradient across said column in the substantial absence of a pressure gradient to induce electroosmotic bulk flow therethrough in a second direction opposite to said first direction, under conditions promoting desorption of said analyte from said adsorption medium; and

(c) recovering mobile phase leaving said adsorption medium due to said electroosmotic bulk flow, said mobile phase containing said analyte.

2. A method in accordance with claim 1 in which said adsorption medium is comprised of particulate solids.

3. A method in accordance with claim 1 further comprising:

(a) passing a wash solution through said adsorption medium between steps (a) and (b) to remove therefrom solutes which chromatographically interfere with said analyte.

4. A method in accordance with claim 1 in which said suspected analyte is present in said source solution at a concentration of less than about 100 μ

g/mL.

5. A method in accordance with claim 1 in which said suspected analyte is present in said source solution at a concentration of less than about 50 μ

g/mL.

6. A method in accordance with claim 1 in which said suspected analyte is present in said source solution at a concentration of less than about 20 μ

g/mL.

7. A method in accordance with claim 1 in which said suspected analyte has a pK_a of from about 6.5 to about 7.5, and said adsorption medium has a surface with substantially non-polar functional groups.

8. A method in accordance with claim 7 in which step (a) includes passing through said adsorption medium a first mobile phase which is substantially polar relative to said adsorption medium, and step (b) includes passing through said adsorption medium a second mobile phase of polarity substantially lower than said first mobile phase.

9. A method in accordance with claim 1 in which said conditions under which step (a) is performed differ from said conditions under which step (b) is performed at least in part by the use of different mobile phases.

10. A method in accordance with claim 9 in which step (a) includes passing a first mobile phase through said adsorption medium, and step (b) includes passing a second mobile phase through said adsorption medium, and said method further comprises filling said adsorption medium with said second mobile phase prior to said (b).

11. A method in accordance with claim 9 in which said different mobile phases differ at least in part according to degree of polarity.

12. A method in accordance with claim 9 in which step (a) includes passing a first mobile phase through said adsorption medium, and step (b) includes passing a second mobile phase through said adsorption medium, said adsorption medium having a polarity which is substantially less than the polarity or said first mobile phase.

13. A method in accordance with claim 9 in which step (a) includes passing a first mobile phase through said adsorption medium, and step (b) includes passing a second mobile phase through said adsorption medium, said adsorption medium having a polarity which is substantially less than the polarity of said first mobile phase, and said second mobile phase having a polarity which is substantially less than the polarity of said first mobile phase.