Title:
Improvement of solid phase microextraction fiber assembly and interface for liquid chromatography.

Abstract:
Modifications were made on commercial SPME fiber assembly and SPME-LC interface to improve the applicability of SPME for LC. Polyacrylonitrile (PAN)/C18 bonded fuse silica was used as the fiber coating for LC applications because the fiber coating was not swollen in common LC solvents at room temperature. The inner tubing of SPME fiber assembly was replaced with a 457 μm outside diameter (o.d.) solid nitinol rod. And the coated fiber (o.d. 290 μm) was installed onto the nitinol rod. The inner diameter (i.d.) of the through hole of the ferrule in the SPME-LC interface was enlarged to 508 μm to accommodate the nitinol rod. The much larger inner rod protected the fiber coating from being stripped when the fiber was withdrawn from the SPME-LC interface. The system was evaluated in term of pressure test, desorption optimization, peak shape, carryovers, linear range, precision, and limit of detection (LOD) with polycyclic aromatic hydrocarbons (PAHs) as the test analytes. The results demonstrated that the improved system was robust and reliable. It overcame the drawbacks, such as leak of solvents and damage of fiber coatings, associated with current SPME fibers and SPME-LC interface. Another sealing mechanism was proposed by sealing the nitinol rod with a specially designed poly(ether ether ketone) (PEEK) fitting. The device was fabricated and tested for manual use.