Nickel–aluminum layered double hydroxide as a nanosorbent for selective solid-phase extraction and spectrofluorometric determination of salicylic acid in pharmaceutical and biological samples

The nickel–aluminum layered double hydroxide (Ni–Al LDH) was synthesized by a simple co-precipitation method and used as a solid-phase extraction (SPE) sorbent for separation and pre-concentration of trace levels of salicylic acid (SA) from aqueous solutions. Extraction of analyte is based on the adsorption of salicylate ions on the Ni–Al (NO3−) LDH and/or their exchanging with LDH interlayer NO3− ions. The retained analyte on the LDH was stripped by 3 mol L−1 NaOH solution and its concentration was subsequently determined spectrofluorometrically at λem = 400 nm with excitation at λex = 270 nm. Various parameters affecting the extraction efficiency of SA on the Ni–Al (NO3−) LDH, such as pH, amount of nano-sorbent, sample loading flow rate, elution conditions, sample volume and matrix effects were investigated. In the optimum experimental conditions, the limit of detection (3 s) and enrichment factor were 0.12 μg L−1 and 40, respectively. The relative standard deviation (RSD) for six replicate determinations of 10 μg L−1 SA was 2.3%. The calibration graph using the pre-concentration system was linear in the range of 0.3–45 μg L−1 with a correlation coefficient of 0.9985. The optimized method was successfully applied to the determination of SA in blood serum, willow leaf and aspirin tablet.