Simultaneous extraction of 32 polychlorinated biphenyls by using magnetic carbon nanocomposite based dispersive microextraction, subsequent dispersive liquid-liquid microextraction with two miscible stripping solvents, and quantitation by GC-μECD.

A highly sensitive new method is described for performing dispersive microextractions. It is making use of a magnetic carbon nanocomposite and two miscible organic solvents. The method was applied to simultaneous extraction of 32 polychlorinated biphenyls (PCBs) prior to their quantitation by gas chromatography with electron capture detection. The effects of pH value of sample for both micro solid phase extraction and dispersive liquid-liquid microextraction, of the amount of sorbent, extraction time, type and volume of the miscible organic solvents and of salt addition were optimized. Figures of merit obtained under optimized conditions (sample solution: 500 ml, volume of disperser solvent, ACN, 1.5 mL; volume of extraction solvent, TCB, 30 μL; extraction time: 50 min, 20 mg magnetic sorbent, centrifuge, 5 min, 4000 rpm), include (a) preconcentration factors between 10,880 and 34,000; (b) repeatabilities of ≤14.9%, (c) detection limits between 0.01 and 0.2 ng kg-1, and (d) linear dynamic ranges from 0.05 to 100 ng kg - 1. The method was applied to the simultaneous analysis of residues in (spiked) real samples of fish, milk, packing sheet, and tap waters. Some of the analytes were found to be present in fish samples. The method is simple, rapid, and more sensitive than any of the previously reported ones. Graphical abstract Schematic presentation of simultaneous extraction of 32 polychlorinated biphenyls (PCBs) by using magnetic carbon nanocomposites (MCNs) based dispersive microextraction (M-SPE), subsequent dispersive liquid-liquid microextraction (DLLME) with two miscible stripping solvents, and quantitation by GC-μECD.