Metal oxide-based electrocatalysts have become increasingly popular in the electrochemical field due to their outstanding electrocatalytic properties. Herein, a hydrothermal approach is used to synthesize the composite of ytterbium zinc oxide endorsed on 2D hexagonal boron nitride (YbZnO@h-BN). Different analytical methods, including Fourier transform infrared (FTIR), Raman spectroscopy, field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD), along with X-ray photoelectron spectroscopy (XPS), are used to interrogate the morphological and structural characteristics of the nanocomposite. FTIR analysis reveals Zn–O and Yb–O functionality, while SEM images shows the YbZnO@h-BN microspherical structure. Cyclic voltammetry (CV) and square-wave voltammetry (SWV) techniques are employed for the electrochemical analysis of Ciprofloxacin (CIP) on the YbZnO@h-BN/glassy carbon electrode (GCE)-modified electrode. The YbZnO@h-BN/GCE sensor demonstrates a broad linear range (0.05 μM to 100 μM) with a lower limit of detection (0.059 μM) and high sensitivity of 7.4441 μA μM⁻¹ cm⁻² under optimal conditions. Additionally, the sensor shows good responsiveness for CIP, along with notable reproducibility, stability, and selectivity. Furthermore, the genuine real wastewater sample and commercial CIP tablet are utilized to investigate the usefulness of the proposed YbZnO@h-BN/GCE sensor for CIP detection in real practice, revealing satisfactory recovery values of 94 to 105% and 95 to 112%, respectively.