The layered chalcogenide has been shown to efficiently absorb organic pollutant, as well as heavy metals and radioactive ions. Previous studied showed that the regeneration of spent layered chalcogenide was impossible because of the strong affinity between soft metal ions and sulfur ions. While can adsorbent of layered chalcogenide be regenerated for adsorption of organic pollutant? In this study a case study of norfloxacin (NOR) adsorbed by layered chalcogenide in water is illustrated. The typical layered chalcogenide, K_1.9Mn_0.95Sn_2.05S₆ (KMS-1) was hydrothermally synthesized and then used to remove NOR in aqueous solution. The adsorption process was found strongly pH-dependent. The maximum adsorption capacities were obtained at pH of 4 at different temperatures. The shift of Bragg peaks indicated from XRD patterns at different pH accompanying SEM images and adsorption amount showed that cation exchange played an essential role to remove NOR. The intercalation of cationic NOR took titled orientations of di-molecular NOR in KMS-1 with the interlayer space of 1.38 nm and 0.97 nm, respectively. The KMS-1 intercalated with NOR can be successfully regenerated by cation exchange using high concentration (1.0 M) KCl solution, in which the decrease in adsorption capacity was found <10% after three adsorption – desorption cycles. The obtained results suggested layered chalcogenide could be a promising regenerated adsorbent to remove organic pollutant with potential application in the environmental remediation.