The aim of the present study is the preparation of a carboxylic acid calix[4]arene-based sorbent. To this end, calix [4]arene containing two carboxylic acid groups in lower rim (ACA) was successfully synthesized and then intercalated between Mg/Al layered double hydroxide (LDH) as a new sorbent (ACA-LDH). The extraction capability of the prepared sorbent was investigated by using the pack column strategy for the extraction of selected nonsteroidal anti-inflammatory drugs (NSAIDs) includes aspirin, ibuprofen and naproxen (as model compounds) from different complicated matrices, as well as ACA and LDH as a control. The successful synthesis of the sorbent was approved using 1H and 13C NMR, FT-IR spectroscopy, MAP, TGA, FE-SEM and XRD. A response surface methodology (RSM) including Plackett–Burman design (PBD) and Box–Behnken design (BBD) were used to refine and optimize parameters affecting extractionand desorption process. The extracted analytes were analyzed using a high-performance liquid chromatography equipped with UV detector (HPLC-UV). Under optimal condition, the response to NSAIDs in the concentration range of 0.5–500 μg.L 1 is linear. The intra-day and inter-day RSDs, and LODs, are <3.5 % and <0.39 μg L 1, respectively. This method was used to successfully identify NSAIDs in human urine samples. The spiking recovery for spiked samples ranged from 91.9 % to 98.5 %. The findings showed that this new sorbent and current procedure could be useful for sensitive, facile and costeffective determining NSAIDs in real samples.
