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Abstract
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Background: Solid-phase microextraction (SPME) is a versatile sampling and sample preparation technology that
possess a significant application in the extraction and pre-concentration of a broad range of micro-pollutants from
different kind of matrices. Selection and preparation of an appropriate fiber substrate and coating materials have
always been the main challenges of the SPME procedure. This paper introduces a high-efficiency metal-based SPME
fiber with a new chemical coating of nickel/graphene oxide/nickel tetraazamacrocyclic complex (Ni/GO/NiTAM).
Result: The Ni/GO/NiTAM sorbent was electroless deposited onto the surface of an aluchrom (Alu) wire, and then the
prepared fiber was employed for the extraction and pre-concentration of some PAHs before their HPLC–UV analysis. The prepared fiber characterization data were assessed using FE-SEM, EDX, XRD, FT-IR, and BET techniques. The
method validation parameters, including the linearity range (LRs: 0.10 to 200.0 µg L−1), the limit of detection (LODs:
0.03‒0.30 µg L−1), and the limit of quantification (LOQs: 0.10–1.00 µg L−1), under optimal conditions. The relative
standard deviations (RSDs) of intra-day, inter-day, and single fiber repeatability (for the samples spiked at 25 µg L‒1)
were in the range of 0.32–2.94, 1.20–4.09, and 1.42‒4.39%, respectively. In addition, the technique recoveries (RR %)
and enrichment factors (EF) were in the range of 83.10‒107.80% and 83–164, respectively.
Conclusion: The fiber fabrication was simple, and the applied materials were also economical and easily accessible.
Alu metal has high physicochemical and mechanical stability and thus can be a good alternative for the substrate of
the fragile commercial SPME fibers. High rigidity and durability, long service life, and high extraction capability are
some of the other advantages of the offered fiber.
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