US4544485A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Chromatographic method and means
Assignee: Purdue Research Foundation
•
Filing: 1984-08-31
•
Granted: 1985-10-01
•
Expires: 2004-08-31
Abstract
Abstract A novel packing material is provided for liquid chromatographic columns, having a maximum pore size around 80 angstroms, a hydrophobic coating on the inner surfaces adapted to absorb hydrophobic analytes, and a hydrophilic coating on the outer surfaces adapted to reject proteins in the analyte sample. A novel method is provided for making the packing material, wherein the packing base is coated, inside and out, with a hydrophilic substance, a hydrophobic substance is bonded to the hydrophilic substance, and the hydrophobic substance is selectively removed from the external surfaces by treatment with an enzyme of a size too large to penetrate into the pores.
Inventors
- 👤 Thomas C. Pinkerton
- 👤 Helene I. Hagestam
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-24 06:21
CPC Classifications
B; B01; B01J; B01J20/00; B01J20/281; B01J20/286; B01J20/287; B01J20/02; B01J20/10; B01J20/103; B01J20/28; B01J20/28002; B01J20/28004; B01J20/28054; B01J20/28078; B01J20/288; B01J20/30; B01J20/3092; B01J20/32; B01J20/3202; B01J20/3204; B01J20/3214; B01J20/3217; B01J20/3231; B01J20/3242; B01J20/3244; B01J20/3246; B01J20/3248; B01J20/3251; B01J20/3253; B01J20/3285; B01J2220/00; B01J2220/50; B01J2220/54; B01J2220/58
Claims Analysis
Total Claims: 22
Claim 1
Independent Claim
87 words
An internal surface reverse phase packing material for liquid chromatographic columns which comprises a porous support having a pore size sufficiently small to prevent the entry of proteinaceous materials into the said packing material, a hydrophobic partitioning phase bonded only to the internal surface thereof, and a hydrophilic partitioning phase bonded to the external surface thereof, whereby proteinaceous substances in an analyte mixture are rejected by the said packing material, while hydrophobic components of the said analyte mixture are adsorbed and retained in the said packing material.
Claim 2
Dependent Claim
87 words
An internal surface reverse phase packing material for liquid chromatographic columns which comprises a porous support having a pore size sufficiently small to prevent the entry of proteinaceous materials into the said packing material, a hydrophobic partitioning phase bonded only to the internal surface thereof, and a hydrophilic partitioning phase bonded to the external surface thereof, whereby proteinaceous substances in an analyte mixture are rejected by the said packing material, while hydrophobic components of the said analyte mixture are adsorbed and retained in the said packing material.
Claim 3
Dependent Claim
13 words
The packing material of claim 1 wherein the said porous support is silica.
Claim 4
Dependent Claim
13 words
The packing material of claim 1 wherein the said porous support is glass.
Claim 5
Dependent Claim
19 words
The packing material of claim 1 wherein the pore size is equal to or less than about 80 angstroms.
Claim 6
Dependent Claim
16 words
The packing material of claim 1 wherein the pore size is less than about 40 μm.
Claim 7
Dependent Claim
16 words
The packing material of claim 1 wherein the particle size is less than about 10 μm.
Claim 8
Dependent Claim
20 words
The packing material of claim 1 wherein the said hydrophilic partitioning phase is comprised of glyceroylpropyl groups bonded to silica.
Claim 9
Dependent Claim
23 words
The packing material of claim 1 wherein the said hydrophobic partitioning phase is composed of polypeptide groups bonded through glyceroylpropyl groups to silica.
Claim 10
Dependent Claim
13 words
The packing material of claim 8 wherein the said polypeptide groups are glycine-L-phenylalanine.
Claim 11
Dependent Claim
13 words
The packing material of claim 8 wherein the said polypeptide groups are glycine-L-phenylalanine-L-phenylalanine.
Claim 12
Independent Claim
97 words
A method for making an internal surface reverse phase packing material for liquid chromatographic columns, which comprises bonding to internal and external surfaces of a porous support a hydrophilic partitioning phase, whereby the pore diameter of the porous support is reduced to a size sufficiently small to prevent the entry of proteinaceous materials into the said packing material, bonding to the said hydrophilic partitioning phase on the internal and external surfaces of the said porous support a hydrophobic partitioning phase, and enzymatically removing the said hydrophobic partitioning phase from the external surface of the said porous support.
Claim 13
Independent Claim
97 words
A method for making an internal surface reverse phase packing material for liquid chromatographic columns, which comprises bonding to internal and external surfaces of a porous support a hydrophilic partitioning phase, whereby the pore diameter of the porous support is reduced to a size sufficiently small to prevent the entry of proteinaceous materials into the said packing material, bonding to the said hydrophilic partitioning phase on the internal and external surfaces of the said porous support a hydrophobic partitioning phase, and enzymatically removing the said hydrophobic partitioning phase from the external surface of the said porous support.
Claim 14
Independent Claim
96 words
A method for making an internal surface reverse phase packing material for liquid chromatogrpahic columns, starting with a porous support having a pore diameter of a size sufficiently small to prevent the entry of proteinaceous materials into the said packing material, and having a hydrophilic partitioning phase bonded to the internal and external surfaces thereof, which comprises bonding to the said hydrophilic partitioning phase on the internal and external surfaces of the said porous support a hydrophobic partitioning phase, and enzymatically removing the said hydrophobic partitioning phase from the external surface of the said porous support.
Claim 15
Independent Claim
96 words
A method for making an internal surface reverse phase packing material for liquid chromatogrpahic columns, starting with a porous support having a pore diameter of a size sufficiently small to prevent the entry of proteinaceous materials into the said packing material, and having a hydrophilic partitioning phase bonded to the internal and external surfaces thereof, which comprises bonding to the said hydrophilic partitioning phase on the internal and external surfaces of the said porous support a hydrophobic partitioning phase, and enzymatically removing the said hydrophobic partitioning phase from the external surface of the said porous support.
Claim 16
Dependent Claim
18 words
The method of claim 11 wherein the said hydrophilic partitioning phase is composed of bound organic hydroxyl groups.
Claim 17
Dependent Claim
19 words
The method of claim 11 wherein the said hydrophilic partitioning phase is composed of glyceroylpropyl groups bonded to silica.
Claim 18
Dependent Claim
22 words
The method of claim 11 wherein the said hydrophobic partitioning phase is composed of polypeptide groups bonded through glyceroylpropyl groups to silica.
Claim 19
Dependent Claim
12 words
The method of claim 15 wherein the said polypeptide groups are glycine-L-phenylalanine.
Claim 20
Dependent Claim
12 words
The method of claim 15 wherein the said polypeptide groups are glycine-L-phenylalanine-L-phenylalanine.
Claim 21
Dependent Claim
27 words
The method of claim 11 wherein the said hydrophobic partitioning phase is removed from the external surface of the said porous support by treatment with carboxypeptidase A.
Claim 22
Dependent Claim
26 words
The method of claim 11 wherein the said hydrophobic partitioning phase is removed from the external surface of the said porous support by treatment with chymotrypsin.
References Cited (Backward Citations)
US3598245A
Cited
US3917527A
Cited
US4061591A
Cited
US4340483A
Cited
US4298500A
Cited
US4376047A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1988-09-30 | 1989-04-01 | 1989-10-01 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1992-09-30 | 1993-04-01 | 1993-10-01 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1996-09-30 | 1997-04-01 | 1997-10-01 | $7700.00 | Window Closed / Lapsed |