Superpolar chromatographic stationary phases and extraction sorbents and their methods of synthesis

• US 9,700,872 B1
• Filed: 07/01/2016
• Issued: 07/11/2017
• Est. Priority Date: 07/01/2016
• Status: Active Grant

• Current Assignee: The Florida International University Board of Trustees (State University System of Florida)
• Original Assignee: The Florida International University Board of Trustees (State University System of Florida)
• Inventors: Kabir, Abuzar, Furton, Kenneth G.
• Primary Examiner(s): Drodge, Joseph
• Application Number:
  US15/200,224
• Time in Patent Office: 375 Days
• Field of Search: 2101982, 21050021, 21050025, 21050027, 2105021, 210511, 210656, 502401, 502405, 502407, 502411, 502414, 96 4, 96 14, 96101, 96108
• CPC Class Codes: B01D 15/22 relating to the construction of the column
• CPC Class Codes: B01D 15/3804 Affinity chromatography
• CPC Class Codes: B01D 15/3885 Using electrical or magnetic means
• CPC Class Codes: B01D 53/04 with stationary adsorbents B01D53/025 takes precedence
• CPC Class Codes: B01D 59/26 by sorption, i.e. absorption, adsorption, persorption
• CPC Class Codes: B01D 71/027 Silicium oxide
• CPC Class Codes: B01D 71/08 Polysaccharides
• CPC Class Codes: B01D 71/702 Polysilsesquioxanes or combination of silica with bridging organosilane groups
• CPC Class Codes: B01J 20/264 derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
• CPC Class Codes: B01J 20/28042 Shaped bodies; Monolithic structures
• CPC Class Codes: B01J 20/28047 Gels
• CPC Class Codes: B01J 20/28097 being coated, filled or plugged with specific compounds
• CPC Class Codes: B01J 20/285 based on polymers
• CPC Class Codes: B01J 20/288 Polar phases
• CPC Class Codes: B01J 20/3085 Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
• CPC Class Codes: B01J 20/3204 Inorganic carriers, supports or substrates
• CPC Class Codes: B01J 20/3242 Layers with a functional group, e.g. an affinity material, a ligand, a reactant or a complexing group
• CPC Class Codes: B01J 20/3272 Polymers obtained by reactions otherwise than involving only carbon to carbon unsaturated bonds
• CPC Class Codes: B01J 2220/54 Sorbents specially adapted for analytical or investigative chromatography
• CPC Class Codes: B01J 2220/86 Sorbents applied to inner surfaces of columns or capillaries
• CPC Class Codes: G01N 2030/025 : Gas chromatography

Abstract

A superpolar sorbent network is a sol-gel network of at least one metal oxide precursor condensed and at least one polyhydroxy molecule. The metal oxide precursor is a silicate precursor, aluminate precursor, titanate precursor, zirconate precursor, germinate precursor, or any combinations thereof, and the polyhydroxy molecule has a multiplicity of hydroxyl groups. The polyhydroxy molecule can be an organic molecule derived from nature. The superpolar sorbent network can be used as a particulate or bulk sorbent for sampling or removal of analytes or contaminants from an environment or can be coated on a tube or particulate substrate for use as a chromatographic stationary phase.

Claims

1. A superpolar sorbent network, comprising a sol-gel network of at least one metal oxide precursor condensed with at least one polyhydroxy molecule where the network comprises units with metal-oxygen-metal groups and units with metal-oxygen-carbon groups respectively bonded to the at least one polyhydroxy molecule of one or more of the structures:

2. The superpolar sorbent network according to claim 1, wherein the metal oxide precursor is a tetraalkoxysilane, trialkoxysilane, or a combination of at least one of the tetraalkoxysilane and trialkoxysilane with a dialkoxysilane.

3. The superpolar sorbent network according to claim 1, wherein the another organic molecule is Sucrose-6-phosphate, Sucrose6F-phosphate, 2-Cyanoethylsucrose, Sucralose, 1-Ketose, UDP-alpha-D-glucose, Uridine Diphosphate Glucose, Sorbitol, or any mixture thereof.

4. The superpolar sorbent network according to claim 1, wherein the metal oxide precursor is tetramethoxysilane and the polyhydroxy molecule comprises sucrose.

5. The superpolar sorbent network according to claim 1, wherein the metal oxide precursor is methyltrimethoxysilane and the polyhydroxy molecule comprises sucrose.

6. The superpolar sorbent network according to claim 1, wherein the at least one metal oxide precursor includes an unsubstituted or substituted arytrialkoxysilane.

7. The superpolar sorbent network according to claim 1, wherein the at least one metal oxide precursor includes an unsubstituted or substituted alkyltrialkoxysilane.

8. A sampling device or analytical device comprising a superpolar sorbent network according to claim 1, wherein the sampling device is an extraction device or a chromatography device.

9. The sampling device or analytical device according to claim 8, wherein the extraction device is a fiber superpolar microextraction fiber, superpolar microextraction tube, superpolar microextraction membrane, superpolar microextraction stir bar, superpolar microextraction fabric, superpolar microextraction capsule, or superpolar microextraction vial.

10. The sampling device or analytical device according to claim 8, wherein the extraction device is a solid phase extractor selected from a matrix solid phase dispersant, a magnetic solid phase extractor, or a dynamic fabric phase sorptive extractor.

11. The sampling device or analytical device according to claim 8, wherein the analytical device is a gas chromatograph or a liquid chromatograph.

12. A method of preparing a superpolar sorbent network according to claim 1, comprising:

providing at least one metal oxide precursor;

providing at least one polyhydroxy molecule;

providing water;

providing a catalyst;

optionally, providing a solvent;

combining the at least one metal oxide precursor, the at least one polyhydroxy molecule, the water, the catalyst, and, optionally, the solvent to form a sol;

hydrolyzing the sol, wherein the at least one metal oxide precursors form hydrolyzed metal oxide precursors; and

condensing the hydrolyzed metal oxide precursors and the at least one polyhydroxy molecules to form a gel that provides the superpolar sorbent network.

13. The method according to claim 12, wherein condensing occurs with heating of the sol.

14. The method according to claim 12, further comprising coating the sol on a substrate, wherein the superpolar sorbent network comprises a coating on the substrate.

15. The method according to claim 14, wherein the substrate is a metal oxide particle, a metal tube, a silica fiber, a fabric, a glass tube, a glass sheet, or a vial.