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 NaHCO 3 -H 2 O 2 . To validate the capability of the CL reaction for pharmaceutical analysis, the CL reaction of β-MnOOH NPLs-NaHCO 3 -H 2 O 2 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-NaHCO 3 -H 2 O 2 CL reaction by the antibiotics. Calibration curves were linear in the range 3.00 Â 10 À5 to 1.00 Â 10 À3 mol L À1 for AMX and in the range 1.00 Â 10 À5 to 1.00 Â 10 À4 mol L À1 for SLB. The limits of detections obtained using the CL method for AMX and SLB were 8.90 Â 10 À6 mol L À1 and 5.60 Â 10 À6 mol L À1 , respectively. The relative standard deviations for AMX and SLB, at the 5.00 Â 10 À5 mol L À1 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.Manganese can construct multiple bonds with oxygen via spontaneous oxidation to form various oxides, hydroxides, and oxyhydroxides, commonly referred to as 'manganese oxides'. [1] Manganese oxides have more than 30 types of crystal structures in different oxidation states of magnesium from +2 to +7. [2] In addition to their high structural versatility, manganese oxides are inexpensive, biocompatible, and nontoxic materials. Moreover, they are stable in high temperatures, and in acidic and basic environments. These features have made these substances suitable for many applications in the areas of catalysis, [3] batteries, [4] magnetic/MRI materials, [5] water remediation, [6] and supercapacitors, [7] among others.MnOOH, a metastable polymorph of trivalent manganese oxyhydroxide, exists in various forms, including α-MnOOH (groutite), β-MnOOH (feitknechtite), and γ-MnOOH (manganite). [8] Structurally, β-MnOOH (feitknechtite) is made of layers of a (Mn 3+ O 6 ) 9À octahedral that lacks interlayer cations. [9] Analytical methods based on chemiluminescence (CL) reactions usually bear good analytical figures of merit. In addition, compared with other luminescence-based techniques such as fluorescence and phosphorescence, the CL methods use simpler and cheaper devices due to the lack of an external light source and monochromator.Amidst CL reactions used for analytical purposes, the reaction of H 2 O 2 -NaHCO 3 is a cost-effective reaction that can be carried out by easily accessible substances. However, the low light intensity of the