Optical fiber technology, in association with the phenomenon of surface plasmon resonance (SPR), has opened a new gateway for quick, easier, and accurate sensing of various chemical, biochemical, and biological parameters. Continuous efforts can be seen in the direction of increasing the sensitivity of the optical fiber biosensors; thus, many hybrid nanostructured optical fiber biosensors composing different nanomaterials, nanomaterial combinations, and different 2D materials have been proposed in the past few decades. This paper discusses the synthesis, characterization, and applications of nanoparticles to the most favorable noble metal for SPR biosensing, i.e., gold. The gold nanoparticles (AuNPs) were prepared by the Turkevich method, and the optical property of AuNPs was characterized using the UV-visible spectrophotometer and transmission electron microscopy (TEM) technique. In addition, the synthesis, characterization, and application of the oxide form the most explored 2D material, i.e., graphene, are also presented in this paper. The graphene oxide was synthesized using an easier and economical method, i.e., a modified Hummer’s method, and an evaluation of the characteristics has been done by a UV-visible spectrophotometer and TEM results.

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