Protective coating and hyperthermal atomic oxygen texturing of optical fibers used for blood glucose monitoring

• US 7,382,944 B1
• Filed: 07/14/2006
• Issued: 06/03/2008
• Est. Priority Date: 07/14/2006
• Status: Expired due to Fees

• Current Assignee: The United States of America As Represented By The Secretary of Agriculture
• Original Assignee: The United States of America As Represented By The Secretary of Agriculture
• Inventors: Banks, Bruce A.
• Primary Examiner(s): Connelly-Cushwa; M. R.
• Assistant Examiner(s): Peace; Rhonda S
• Application Number:
  US11/489,813
• Time in Patent Office: 690 Days
• Field of Search: 385/12, 385/37, 385/38
• US Class Current: 385/12
• CPC Class Codes: G01N 2021/7706 Reagent provision
• CPC Class Codes: G01N 21/7703 using reagent-clad optical fibres or optical waveguides using measurement of total internal reflection or attenuated total reflection G01N21/552; optical fibres or waveguides per se G02B
• CPC Class Codes: G02B 6/02309 Structures extending perpendicularly or at a large angle to the longitudinal axis of the fibre, e.g. photonic band gap along fibre axis
• CPC Class Codes: G02B 6/02395 Glass optical fibre with a protective coating, e.g. two layer polymer coating deposited directly on a silica cladding surface during fibre manufacture G02B6/02052, G02B6/02057, G02B6/024, G02B6/032, G02B6/105, G02B6/14 take precedence; coating on fibre gratings G02B6/02104; multilayer core or cladding G02B6/036; reinforcing splice joints G02B6/2558; optical cables, i.e. comprising protective structures external to the protective coating such as a jacket or plural coated optical fibres G02B6/44; coating of glass to obtain optical fibres C03C25/104

Abstract

Disclosed is a method of producing cones and pillars on polymethylmethacralate (PMMA) optical fibers for glucose monitoring. The method, in one embodiment, consists of using electron beam evaporation to deposit a non-contiguous thin film of aluminum on the distal ends of the PMMA fibers. The partial coverage of aluminum on the fibers is randomly, but rather uniformly distributed across the end of the optical fibers. After the aluminum deposition, the ends of the fibers are then exposed to hyperthermal atomic oxygen, which oxidizes the areas that are not protected by aluminum. The resulting PMMA fibers have a greatly increased surface area and the cones or pillars are sufficiently close together that the cellular components in blood are excluded from passing into the valleys between the cones and pillars. The optical fibers are then coated with appropriated surface chemistry so that they can optically sense the glucose level in the blood sample than that with conventional glucose monitoring.

Claims

1. A sensor comprising a single solid light-conducting fiber having a textured surface site consisting of a textured distal end first having a non-contiguous protective coating deposited thereon which is treated by being placed in a vacuum and then subject to directed hyperthermal beams comprising oxygen ions or atoms, wherein said textured distal end comprises said non-contiguous protective coating thereon and cones separated from each other by an amount which is about 1 micron.

2. The sensor according to claim 1, wherein said protecting coating is of a material selected from the group comprising aluminum, gold, silicon dioxide and sodium chloride.

3. The sensor according to claim 2, wherein said aluminum has a thickness in the range from about 10 microns to about 500 microns.

4. The sensor according to claim 1, wherein said single solid light-conducting fiber has a diameter in the range from about 1.0 mm to about 2.0 mm.

5. The sensor according to claim 1, wherein said textured distal end comprises cones having a length to width ratio, which is greater than one.

6. The sensor according to claim 5, wherein said cones have a conical shape.

7. The sensor according to claim 1, wherein an analyte-responsive reagent is deposited on said fiber at said textured surface site.

8. The sensor according to claim 1, wherein said light-conducting fiber is transparent and is of polymer material except for silicone.

9. The sensor according to claim 8, wherein said light-conducting fiber is polymethylmethacralate.

10. A method of producing a solid light-conducting fiber used in the analysis of a blood comprising the steps of:

a) selecting at least one single solid light-conducting fiber having a point of attachment and a distal end;

b) depositing a protective coating on said distal end of said at least one light-conducting fiber;

c) placing said at least one light-conducting fiber having said protective coating on said distal end in a vacuum source; and

d) subjecting said distal end to directed hyperthermal beams comprising oxygen ions or atoms.

11. The method according to claim 10, wherein said protective coating is of a material selected from the group comprising aluminum, gold, silicon dioxide, and sodium chloride.

12. The method according to claim 11, wherein said aluminum has a thickness in the range from about 10 microns to about 500 microns.

13. The method according to claim 10, wherein said single light-conducting fiber is polymethylmethacralate.

14. The method according to claim 10, wherein said single solid light-conducting fiber has a diameter in the range from about 1.0 mm to about 2.0 mm.

15. The method according to claim 10, wherein said vacuum source supplies a pressure of less than about 1×

10<sup>−

5</sup> while said distal end is being subjected to said directed hyperthermal beams comprising ions or atoms.

16. The method according to claim 10, wherein said directed hyperthermal beams have an energy level that is in the range from about greater than 1 eV to about 100 eV.

17. The method according to claim 16, wherein said directed hyperthermal beams is in the range from about 30 eV to about 150 eV.

18. The method according to claim 10, wherein said directed hyperthermal beams comprising oxygen ions or atoms are provided from a source selected from the group consisting of an End Hall source, an electron bombardment ion source, a microwave plasma source and an arc source.

19. The method according to claim 18, wherein said selected source and said distal end are spaced apart from each other by a distance in the range from about 3 cm to about 200 cm.

20. The method according to claim 19, wherein said at least one solid light-conducting fiber comprises a plurality arranged in a bundle and each having a distal end.

21. The method according to claim 20, wherein said selected source and said bundle has a shield interposed therebetween and wherein said selected source and said distal ends of said bundle are spaced apart from each other by a distance in the range from about 3 cm to about 200 cm.

22. The method according to claim 21, wherein said shield is selected from the group consisting of a water-cooled shield and multilayer insulation shield.

23. The method according to claim 18, wherein said source is an End Hall source having a hollow cathode and separated from said distal ends of said bundle by a distance in the range from about 3 cm to about 200 cm.

24. A method of analyzing for an analyte in a fluid comprising the steps of:

providing a single solid light-conducting fiber with a point of attachment and having a distal end with a protective coating deposited thereon and wherein said protective coating is further prepared by being placed in a vacuum and then subjected to directed hyperthermal beams comprising oxygen ions or atoms, said distal end further having an analyte-responsive reagent deposited thereon;

bringing a droplet of the fluid containing said analyte and having an initial sampling volume of less than 5 microliters into contact with said distal end of said site, so as to produce a physical or chemical response by interaction of said reagent with said analyte, said response being detectable by a change in characteristics of a light beam;

transmitting a light beam from a light source into said point of contact and into said distal end; and

analyzing said light beam reflected from said distal end for said change, said change being correlative with presence of said analyte in the fluid.

25. The method according to claim 24, wherein said change is correlative with the concentration of said analyte in the fluid.

26. The method according to claim 25, wherein the fluid being brought into contact with said fiber has an initial sampling volume of about 0.2 to about 0.4 microliters.

27. The method according to claim 26, wherein the fluid is blood and the analyte is glucose.