Chemiluminescence (CL) reactions are chemical reactions releasing energy as electromagnetic emission. Analytical approaches based on CL reactions are usually convenient, economical, and exhibit good figures of merits such as wide linear concentration range and high sensitivity [1]. NiS nanoparticles (NPs) have many utilizations in diverse fields of advanced research like catalysts, cathodes of rechargeable lithium batteries, solar cells, and supercapacitors [2]. In this work, a new and sensitive CL method was proposed for determination of amoxicillin (AMX) and cefazolin (CFZ) in pharmaceutical preparations. The CL method is based on enhancing effect of AMX and quenching effect of CFZ on the NiS NPs- luminol-O2 chemiluminescence (CL) reaction in a strongly alkaline medium. NiS synthesized by hydrothermal synthesis method by X-ray diffraction (XRD), scanning electron microscopy (SEM), and Fourier-transform infrared spectroscopy (FTIR) methods. The effects of various chemical reagents, involved in the CL reaction, on the CL emission intensity were also investigated and optimized. Under the optimum conditions, a linear relationship was obtained between the CL intensity and the concentration of CFZ and AMX in the range of 1.00×10-5- 1.00×10-3 mol L-1 and 1.00×10-6 – 8.00×10-4 mol L-1with limit of detections of 4.5×10-6 and 2.5×10-7 mol L-1, respectively. The mechanism of CL system was also discussed, briefly.
