A fluorescent zinc-based two-dimensional (2D) coordination polymer, {[Zn(cis-CHA)(BPEP)0.5]•DMF}n (ZCP), has been synthesized using solvothermal reaction conditions. ZCP is characterized using singlecrystal X-ray diffraction, powder X-ray diffraction, Fourier-transform infrared spectroscopy, thermogravimetric study, and elemental analysis. In waterdispersed medium, the framework (ZCP) detects antibiotics, such as nitrofurantoin (NFT) and nitrofurazone (NZF), as well as an organo-toxin aromatic compound, trinitrophenol (TNP). The limit of detection (LOD) values for NFT, NZF, and TNP are found to be 21.75, 24.31, and 13.47 ppb, respectively. Such sensing behavior is also apprehended by colorimetric response in solid and solution along with a strip paper method. After sensing of each and individual analytes, the sensor is recycled without losing its efficiency. Interestingly, the detection of these analytes by this sensor is also comprehended for real-field analysis with high accuracy and repeatability. The sensing behavior is strongly supported by profound experimental investigation, including the lifetime measurement, and the mechanism of sensing is well supported by theoretical calculations.