Application of Molecularly Imprinted Solid-Phase Extraction Coupled with HPLC for Preconcentration and Trace Determination of Celecoxib in the Human Urine Samples: Optimization by Central Composite Design (CCD)

Document Type : Research Article

Authors

Department of Chemistry, Islamic Azad University, Saveh Branch, Saveh, I.R. IRAN

Abstract

A Molecularly Imprinted Solid-Phase Extraction (MISPE) coupled with High-Performance Liquid Chromatography with UV detection (HPLC/UV) described for preconcentration and trace determination of celecoxib in human urine samples. The synthesis of the Molecularly Imprinted Polymer (MIP) was performed by a non-covalent approach using methacrylic acid (MAA) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker monomer, chloroform as the solvent, 2,2′-azobisisobutyronitrile (AIBN) as the initiator and celecoxib template as the target drug. Non-molecularly Imprinted Polymer (NIP) was also synthesized for comparison. Scanning Electron Microscopy (SEM) and FT-IR spectroscopy were used for characterizing the synthesized polymers. Also, a Central Composite Design (CCD) under Response Surface Methodology (RSM) and chemometrics applied to investigate and optimize the MISPE procedure parameters such as pH, loading and eluent solvent flow-rate, eluent solvent volume and sorbent mass, that probably influence the extraction process, to achieve the highest celecoxib extraction efficiency. Batch rebinding capacity of celecoxib was determined from the derived Langmuir isotherm and was found to be 15.06 mg/g. The Limit of Detection (LOD) and Limit of Quantification (LOQ) of this proposed method were 8 ng/mL and 26.7 ng/mL, respectively. The recoveries were 92.60-102% and the Relative Standard Deviation (RSD %) was lower than 4.65% in spiked urine samples. Accordingly, the proposed MISPE-HPLC/UV method can be used for the separation of trace amounts of celecoxib in human urine samples.

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