The efficient extraction of tianeptine from environmental matrices has been a matter of concern issue due to the amphiphilic ionic organic substance property of tianeptine. A magnesium-iron layered double hydroxide (Mg/Fe-LDH) was successfully synthesized using hydrothermal synthesis and characterized by X-ray diffraction, Fourier transform infrared spectroscopy, and scanning electron microscopy techniques. The as-prepared nanocomposite was used as an effective adsorbent to extract tianeptine from water samples via a dispersive solid-phase extraction (DSPE) procedure before high-performance liquid chromatography-ultraviolet detection (HPLC-UV). Experimental parameters affecting extraction efficiency, such as agitation type, pH, absorbent amount, elution solvent type, and absorption/elution time, were studied and optimized. The developed tianeptine analysis method, based on adsorption-release extraction using Mg/Fe-LDH and detection by HPLC-UV, exhibited a wide quantitative linear range of 10 to 1000 mu g/L (r(2) = 0.9986, p = 2.49 x 10(-14)) by plotting chromatography peak height versus tianeptine concentration. The limits of detection and quantification were 4.6 and 15 mu g/L, respectively. The developed tianeptine analysis method was applied to analyze tianeptine spiked in water samples. An ideal recovery range of 94.1 to 103.5%, with a narrow relative standard deviation of 1.63-4.34%, was obtained. The proposed analysis method, which combined Mg/Fe-LDH-based DSPE with HPLC-UV detection, was reliable for determining tianeptine in environmental water samples.