Solid-phase microextraction coatings and methods for their preparation

• US 8,598,325 B2
• Filed: 03/05/2012
• Issued: 12/03/2013
• Est. Priority Date: 03/11/2002
• Status: Expired due to Term

• Current Assignee: Janusz B. Pawliszyn
• Original Assignee: Janusz B. Pawliszyn
• Inventors: Pawliszyn, Janusz B.
• Primary Examiner(s): Haq, Shafiqul
• Application Number:
  US13/412,122
• Publication Number:
  US 20120164286A1
• Time in Patent Office: 638 Days
• Field of Search: None
• US Class Current: 530/415
• CPC Class Codes: A61B 10/0045 Devices for taking samples of body liquids devices for taking blood samples A61B5/15
• CPC Class Codes: G01N 1/405 by adsorption or absorption
• CPC Class Codes: G01N 2030/009 Extraction
• CPC Class Codes: G01N 2030/062 extracting sample from raw material
• CPC Class Codes: Y10T 428/2933 Coated or with bond, impregnation or core

Abstract

There is described a coated solid phase microextraction (SPME) fiber for use in direct immersion SPME of a food matrix that includes carbohydrates. The coated SPME fiber includes a SPME fiber for absorbing a small molecule from the food matrix; and a protective coating which has a surface that is substantially uniform and substantially smooth, the protective coating reducing adsorption of the carbohydrates onto the SPME fiber and allowing the SPME fiber to extract the small molecule from the food matrix. A process for producing the coated SPME fiber and a method of performing solid phase microextraction are also described.

Claims

1. A coated solid phase microextraction (SPME) fibre for use in direct immersion SPME of a food matrix that includes carbohydrates, the coated SPME fibre comprising:

a SPME fibre having an extractive portion for absorbing a small molecule from the food matrix; and

a protective coating that comprises polydimethylsiloxane (PDMS) or polyfluorocarbons and that is between about 10 μ

m and about 40 μ

m thick, wherein the protective coating covers the extractive portion of the SPME fiber and wherein the protective coating has an exposed surface that is substantially uniform and substantially smooth, the protective coating reducing adsorption of the carbohydrates onto the SPME fibre and allowing the SPME fibre to extract the small molecule from the food matrix,

wherein the substantially uniform, substantially smooth surface of the protective coating has, on average fewer than 2 imperfections greater than 10 nm in length per 1000 nm² of protective coating, as seen on a 900×

magnification of an Electron Scanning Microscope.

2. The coated SPME fibre according to claim 1, wherein the surface of the protective coating is substantially non-porous.

3. The coated SPME fibre according to claim 1, wherein:

the SPME fibre is a commercially available SPME fibre;

or

the SPME fibre comprises a bonding polymer adhering together SPME particles which have pores for absorbing the small molecule from the food matrix.

4. The coated SPME fibre according to claim 1, wherein

the substantially uniform, substantially smooth surface of the protective coating has, on average:

fewer than 1 imperfections greater than 10 nm in length per 1000 nm² of protective coating, as seen on a 900×

magnification of an Electron Scanning Microscope, or

fewer than 0.1 imperfections greater than 10 nm in length per 1000 nm² of protective coating, as seen on a 900×

magnification of an Electron Scanning Microscope;

or wherein the substantially uniform, substantially smooth surface of the protective coating has no observable imperfections when viewed at 900×

magnification using an Electron Scanning Microscope.

5. The coated SPME fibre according to claim 1, wherein the food matrix is selected from the group consisting of fruit pulp, fruit juice, vegetable pulp, vegetable juice, and any combination thereof.

6. The coated SPME fibre according to claim 1, wherein the small molecule is a hydrophobic or hydrophilic molecule having a molecular mass less than about 10,000 atomic mass units.

7. The coated SPME fibre according to claim 1, wherein the small molecule is a triazole pesticide.

8. A method of direct immersion solid phase microextraction (DI-SPME) of a small molecule from a food matrix that includes carbohydrates, the method comprising:

providing the food matrix;

immersing a coated solid phase microextraction (SPME) fibre according to claim 1 into the food matrix;

removing the coated SPME fibre from the food matrix; and

analyzing the small molecule extracted from the food matrix by chromatography.

9. The method according to claim 8 where the chromatography is gas chromatography.

10. The method according to claim 8, wherein the small molecule is a triazole pesticide.

11. The method according to claim 8, wherein the food matrix is selected from the group consisting of fruit pulp, fruit juice, vegetable pulp, vegetable juice, and any combination thereof.

12. The method according to claim 8, wherein

the substantially uniform, substantially smooth surface of the protective coating has, on average:

fewer than 1 imperfections greater than 10 nm in length per 1000 nm² of protective coating, as seen on a 900×

magnification of an Electron Scanning Microscope, or

fewer than 0.1 imperfections greater than 10 nm in length per 1000 nm² of protective coating, as seen on a 900×

magnification of an Electron Scanning Microscope;

or wherein substantially uniform, substantially smooth surface of the protective coating has no observable imperfections when viewed at 900×

magnification using an Electron Scanning Microscope.

13. The coated SPME fibre according to claim 1, wherein the SPME fiber comprises divinylbenzene as an extractive material.

14. The coated SPME fibre according to claim 1, wherein the protective coating comprises polydimethylsiloxane (PDMS).

15. The coated SPME fibre according to claim 1, wherein the small molecule is selected from the group consisting of:

triadimefon, penconazole, triadimenol, hexaconazole, and diniconazole.