Dual ligand sol-gel sorbent combining superhydrophobicity and π-π interaction

Patent metadata

Field	Value
Publication number	US-10967356-B1
Application number	US-201715813799-A
Country	US
Kind code	B1
Filing date	Nov 15, 2017
Priority date	Nov 15, 2016
Publication date	Apr 6, 2021
Grant date	Apr 6, 2021

Abstract

A dual ligand sol-gel sorbent and method of manufacture is provided herein. The dual ligand sol-gel sorbent provides superior enrichment effects through simultaneous exploitation of superhydrophobicity of one of the ligands and the ability of the other ligand to undergo π-π interaction with hydrophobic aromatic analytes. Sorbent performance is enhanced both in terms of analyte enrichment and sorbent stability, such as pH stability and solvent stability.

First claim

What is claimed is:

1. A dual ligand sol-gel sorbent for use in solid phase microextraction (SPME) comprising:
at least two sol-gel precursors wherein the sol-gel precursors are a perfluorododecyl (PF-C 12 ) ligand and a phenethyl ligand;
an inorganic co-precursor; and
a catalyst wherein the catalyst is trifluoroacetic acid (TFA);
wherein the dual ligand sol-gel provides enhanced extraction capability for aliphatic hydrocarbons, aromatic hydrocarbons, and nonpolar derivatives thereof.

2. The sorbent of claim 1 , wherein the inorganic co-precursor is a germania co-precursor or a silica co-precursor.

3. The sorbent of claim 2 , wherein the silica co-precursor is TMOS.

4. The sorbent of claim 2 , wherein the germania co-precursor is TEOG.

5. The sorbent of claim 4 , wherein the ligands are in equimolar concentration.

6. A method of manufacturing a dual-ligand sol-gel sorbent for use in solid phase microextraction (SPME) comprising steps in the order of:
adding at least two sol-gel precursors to a vial wherein the at least two sol-gel precursors are a perfluorododecyl (PF-C 12 ) ligand and a phenethyl ligand;
adding an inorganic co-precursor to the vial; and
adding a catalyst to the vial to form a solution wherein the catalyst is trifluoroacetic acid (TFA);
wherein selectivity for an analyte in SPME can be controlled by adjusting a ratio of the at least two sol-gel precursors.

7. The method of claim 6 , further comprising mixing the at least two sol-gel precursors after adding the at least two sol-gel precursors to the vial.

8. The method of claim 6 , further comprising mixing the inorganic co-precursor with the at least two sol-gel precursors after adding the inorganic co-precursor to the vial.

9. The method of claim 6 , further comprising mixing the solution after adding the catalyst.

10. The method of claim 6 , wherein the inorganic co-precursor is a germania co-precursor or a silica co-precursor.

11. The method of claim 10 , wherein the silica co-precursor is TMOS.

12. The method of claim 10 , wherein the germania co-precursor is TEOG.

13. The method of claim 6 , wherein the ligands are in equimolar concentration.

Assignees

• Malik Abdul
• Seyyal Emre
• Univ South Florida

Inventors

• Malik Abdul
• Seyyal Emre

Classifications

• C09D183/08 Primary

  containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen · CPC title

• B01J2220/86

  Sorbents applied to inner surfaces of columns or capillaries · CPC title

• B01J20/3285

  Coating or impregnation layers comprising different type of functional groups or interactions, e.g. different ligands in various parts of the sorbent, mixed mode, dual zone, bimodal, multimodal, ionic or hydrophobic, cationic or anionic, hydrophilic or hydrophobic · CPC title

• B01J20/3248

  the functional group or the linking, spacer or anchoring group as a whole comprising at least one type of heteroatom selected from a nitrogen, oxygen or sulfur, these atoms not being part of the carrier as such · CPC title

• B01J20/3246

  having a well defined chemical structure · CPC title