Monolithic graphene fibers for solid-phase microextraction

• Monolithic graphene fiber for SPME.
• Distinguishing advantages of the monolithic fiber over conventional fibers.
• Great potential for practical use.

Monolithic graphene fibers for solid-phase microextraction (SPME) were fabricated through a dimensionally confined hydrothermal strategy and their extraction performance was evaluated. For the fiber fabrication, a glass pipeline was innovatively used as a hydrothermal reactor instead of a Teflon-lined autoclave. Compared with conventional methods for SPME fibers, the proposed strategy can fabricate a uniform graphene fiber as long as several meters or more at a time. Coupled to capillary gas chromatography (GC), the monolithic graphene fibers in a direct-immersion (DI) mode achieved higher extraction efficiencies for aromatics than those for n-alkanes, especially for polycyclic aromatic hydrocarbons (PAHs), thanks to π–π stacking interaction and hydrophobic effect. Additionally, the fibers exhibited excellent durability and can be repetitively used more than 160 times without significant loss of extraction performance. As a result, an optimum extraction condition of 40 °C for 50 min with 20% NaCl (w/w) was finally used for SPME of PAHs in aqueous samples. For the determination of PAHs in water samples, the proposed DI-SPME-GC method exhibited linear range of 0.05–200 μg/L, limits of detection (LOD) of 4.0–50 ng/L, relative standard deviation (RSD) less than 9.4% and 12.1% for one fiber and different fibers, respectively, and recoveries of 78.9–115.9%. The proposed method can be used for analysis of PAHs in environmental water samples.