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In this work,the nickel-aluminum layered double hydroxide(Ni-Al LDH) with nitrate interlayer anion was synthesized and used as a solid phase extraction sorbenl for the selective separation and pre-concentration of mefenamic acid prior to quantification by UV detection at λ_(max)=286 nm.Extraction procedure is based on the adsorption of inefenamate anions on the Ni-Al(NO_3~-) LDH and/or their exchange with LDH interlayer NO_3~- anions.The effects of several parameters such as cations and interlayer anions type in LDH structure.pH,sample flow rate,elution conditions,amount of nano-sorbent and co-existing ions on the extraction were investigated and optimized.Under the optimum conditions,the calibration graph was linear within the range of 2-1000 μg/L with a correlation coefficient of 0.9995.The limit of detection and relative standard deviation were 0.6 μg/L and 0.84%(30 μg/L.n = 6).respectively.The presented method was successfully applied to determine of mefenamic acid in human serum and pharmaceutical wastewater samples.