In this research, β-MnOOH nanoplates (NPLs) were hydrothermally produced and then identified using several spectroscopic methods. The β-MnOOH NPLs were used to catalyze the chemiluminescence (CL) reaction of NaHCO3–H2O2. To validate the capability of the CL reaction for pharmaceutical analysis, the CL reaction of β-MnOOH NPLs-NaHCO3-H2O2 reaction was exploited to develop a new method of measuring antibiotics named amoxicillin (AMX) and salbutamol sulfate (SLB). This method is based on the attenuating β-MnOOH NPLs-NaHCO3-H2O2 CL reaction by the antibiotics. Calibration curves were linear in the range 3.00 10 5 to 1.00 10 3 mol L 1 for AMX and in the range 1.00 10 5 to 1.00 10 4 mol L 1 for SLB. The limits of detections obtained using the CL method for AMX and SLB were 8.90 10 6 mol L 1 and 5.60 10 6 mol L 1, respectively. The relative stan- dard deviations for AMX and SLB, at the 5.00 10 5 mol L 1 concentration, were 2.44% and 2.57% (n = 5), respectively. The study of the effect of foreign species showed that the CL method developed has the appropriate selectivity for AMX and SLB. The success of the CL method in actual samples analysis was demonstrated by accurately measuring the selected antibiotics in the pharmaceutical formulations.