In this article, nickel(II) oxide (NiO) hollow microspheres (HMSs) were fabricated and used to catalyze chemiluminescence (CL) reaction. The studied CL reaction is the luminol-oxygen reaction that was used as a sensitive analytical tool for measuring tuberculostatic drug isoniazid (IND) in pharmaceutical formulations and water samples. The CL method was established based on the suppression impact of IND on the CL reaction. The NiO HMSs were produced by a simple hydrothermal method and characterized by several spectroscopic techniques. The result of essential parameters on the analytical performance of the CL method, including concentrations of sodium hydroxide (NaOH), luminol, and NiO HMSs were investigated. At the optimum conditions, the calibration curve for IND was linear in the range of 8.00 × 10−7 to 1.00 × 10−4 mol L−1 (R2 = 0.99). A detection limit (3S) of 2.00 × 10−7 mol L−1 was obtained for this method. The acceptable relative standard deviation (RSD) was obtained for the proposed CL method (2.63%, n = 10) for a 5.00 × 10−6 mol L−1 IND solution. The mechanism of the CL reaction was also discussed.
