Application of of Fe3O4@SiO2-NH2 for extraction of diclofenac from environmental waters and its determination with HPLC

Diclofenac (DFC) is a non-steroidal antiinflammatory pain reliever drug. It is often used for the treatment of rheumatoid arthritis, ankylosing spondylitis, osteoarthritis, and sports injuries. The determination of the low level of DFC in pharmaceutical and biological samples is very important for medical and pharmaceutical practical aspects where it is used for the treatment of various diseases.The determination of the low level of DFC in pharmaceutical and biological samples is very important for medical and pharmaceutical practical aspects where it is used for the treatment of various diseases [1]. Several methods have been reported for the determination ofdiclofenac in pharmaceutical preparations or biological fluids, suchas high-performance liquid chromatography (HPLC), spectrophotometry, high-performance thin layer chromatography, capillary zone electrophoresis and electrochemical detections [2]. In this work a simple, rapid and novel method for the extraction and preconcentration of DFC in water samples using amino-functionalized Fe3O4@SiO2 core-shell magnetic nanomatrial was developed. The properties of particles were characterized by Transmission electron microscopy transmission Scanning electron microscopy and X-Ray Diffraction. The Fe3O4@SiO2-NH2 particles were successfully applied to simultaneously enrich and separate DFC. The separation was reached in less than 5 min using a C18 column and an isocratic binary mobile phase (acetonitrile: water (70:30, v/v)) with flow rate of 1.0 mL min−1. Influence variables such as pH, Fe3O4@SiO2-NH2, volume of desorption solvent and extraction time were screened. The significant variables were optimized by using acentral composite design (CCD). At optimum conditions values of variables set as pH = 4, 12 mg sorbent, 0.5 mL methanol, and 10 min extraction time