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A layered porous organic framework (L-POF) with high surface area and porous volume was used as a novel adsorbent for adsorption of chlorophenols (CPs). The L-POF showed much higher adsorption capacity for four CPs (2-CP, 3-CP, 2,3-CP, 2,4-CP) compared with corresponding amorphous POF and some commercial adsorbents. Then, an L-POF-based solid-phase extraction method combined with high-performance liquid chromatography for analyzing CPs at the wavelength of 280 nm in water and honey samples was established. Under the optimum conditions,