Cyanogen bromide-activation of hydroxyls on silica for high pressure affinity chromatography

• US 6,375,846 B1
• Filed: 11/01/2001
• Issued: 04/23/2002
• Est. Priority Date: 11/01/2001
• Status: Expired due to Fees

• Current Assignee: Harry Wellington Jarrett, Luis A. Jurado
• Original Assignee: Harry Wellington Jarrett, Luis A. Jurado
• Inventors: Jurado, Luis A., Jarrett, Harry Wellington
• Primary Examiner(s): Therkorn, Ernest G.
• Application Number:
  US09/682,922
• Time in Patent Office: 173 Days
• Field of Search: 210/635, 210/656, 210/198.2, 210/502.1, 502/401, 502/439
• US Class Current: 210/635
• CPC Class Codes: B01J 20/103 comprising silica
• CPC Class Codes: B01J 20/28083 being in the range 2-50 nm, i.e. mesopores
• CPC Class Codes: B01J 20/281 Sorbents specially adapted for preparative, analytical or investigative chromatography
• CPC Class Codes: B01J 20/286 Phases chemically bonded to a substrate, e.g. to silica or to polymers
• CPC Class Codes: B01J 20/3092 Packing of a container, e.g. packing a cartridge or column of chromatography columns B01D15/206
• CPC Class Codes: B01J 20/3204 Inorganic carriers, supports or substrates
• CPC Class Codes: B01J 20/3217 Resulting in a chemical bond between the coating or impregnating layer and the carrier, support or substrate, e.g. a covalent bond
• CPC Class Codes: B01J 20/3219 involving a particular spacer or linking group, e.g. for attaching an active group
• CPC Class Codes: B01J 20/3244 Non-macromolecular compounds
• CPC Class Codes: B01J 20/3257 the functional group or the linking, spacer or anchoring group as a whole comprising at least one of the heteroatoms nitrogen, oxygen or sulfur together with at least one silicon atom, these atoms not being part of the carrier as such
• CPC Class Codes: B01J 20/3259 comprising at least two different types of heteroatoms selected from nitrogen, oxygen or sulfur with at least one silicon atom
• CPC Class Codes: B01J 20/3263 comprising a cyclic structure containing at least one of the heteroatoms nitrogen, oxygen or sulfur, e.g. an heterocyclic or heteroaromatic structure
• CPC Class Codes: B01J 2220/54 Sorbents specially adapted for analytical or investigative chromatography
• CPC Class Codes: B01J 2220/58 Use in a single column

Abstract

The present invention provides for a method to prepare a pressure stable and pH stable medium for use in high pressure (performance) affinity chromatography. The method includes the steps of treating hydroxyalkyl-silica with cyanogen halides or other cyanogen transfer reagents in the presence of an organic base in anhydrous solvents at temperatures in the range of from about −15° C. to about 20° C. for a period of time in the range of from about 1 minute to about 5 minutes, and washing the resulting medium in anhydrous solvent.

Claims

1. A method to prepare a pressure stable and pH stable medium for use in high performance affinity chromatography, the method comprising the steps of treating hydroxyalkyl-silica with cyanogen transfer reagent in the presence of an organic base in anhydrous solvents at temperatures in the range of from about −

15°

C. to about 20°

C. for a period of time in the range of from about 1 minute to about 5 minutes, and washing the resulting medium in anhydrous solvent.

2. The method in claim 1 wherein the hydroxyalkyl-silica is glycidioloxypropyl-silica.

3. The method in claim 1 where the cyanogen transfer reagent is cyanogen bromide.

4. The method in claim 1 where the organic base is triethylamine.

5. The method in claim 1 where the anhydrous solvent is selected from the group consisting of acetone, N,N-dimethylformamide, and 2-propanol.

6. The method in claim 1 where the temperature is about −

15°

C. and the period is about 3 minutes.

7. The method in claim 1 where the temperature is about 20°

C. and the period is about 5 minutes.

8. The method of claim 1 where the cyanogen transfer agent is a cyanogen halide.