Reports the investigation of serum and urine samples of α-chloralose, a compound used as a rodenticide in the control of bird pests, patients by gas chromatography-mass spectrometry (GC-MS ) in the electron impact mode to analyze the [sup1]h nuclear magnetic resonance ([sup1]H NMR) spectroscopy and GC-MS of α-chloralose. Overview of the characterization of α-chloralose species by [sup1]H NMR spectrometry; Highlights of the case histories used in this investigation; Methods used in the detection and quantitation of α-chloralose in biological fluids; Account of [sup1]H NMR analysis performed in this investigation.