Determination of chloramphenicol and tetracycline residues in milk samples by means of nanofiber coated magnetic particles prior to high-performance liquid chromatography-diode array detection.

A magnetic solid phase extraction (MSPE) coupled with high-performance liquid chromatography-diode array detection (HPLC-DAD) methodology was developed for the determination of chloramphenicol (CP) and tetracycline (TET) antibiotic residues in milk samples. As a solid phase sorbent, C-nanofiber coated magnetic nanoparticles were synthesized and extensively characterized using Field Emission Scanning Electron Microscopy (FE-SEM), Raman Spectroscopy and X-ray Powder Diffraction (XRD) analysis. Experimental variables of MSPE method for both antibiotic analytes were investigated and optimized systematically. After MSPE, the linear range for both the analytes (r > 0.9954) were obtained in a range 10.0-600.0 ng mL. The limit of detections (LODs) for CP and TET were 3.02 and 3.52 ng mL, respectively while RSDs % were below than 4.0%. Finally, the developed method based on MPSE-HPLC-DAD was applied to real milk samples to quantify the antibiotic residues. Recovery values for each antibiotic compound were found in the range of 94.6-105.4% (n = 3) by using spiked model solution.