An isonicotinic acid hydrazide (INAH) chemically modified fumed silica, as a novel adsorbent, was designed for the preconcentration and determination of Hg (II) ions in fish samples via the solid phase extraction followed by the hydride generation atomic absorption spectrometry (HG-AAS). In this work, the efficiency of the synthesized adsorbent was investigated to determine its ability for the extraction of the Hg (II) ions from the aqueous solutions. The extraction efficiency was investigated by optimizing of different experimental conditions, such as pH, sample volume, flow rate, adsorbent dosage, and eluent type. Under the optimal conditions, a linear calibration curve for the solid phase extraction method was obtained in the range of between 0.12 and 16.5 μg L. The obtained detection limit and preconcentration factor were 0.018 μg L and 25, respectively (RSD > 3%). The proposed optimized method was successfully applied to fish samples.