Preconcentration of organochlorine pesticides in aqueous samples by dispersive liquid-liquid microextraction based on solidification of floating organic drop after SPE with multiwalled carbon nanotubes

SPE joined with dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) as a novel technique combined with GC with electron-capture detection has been developed as a preconcentration technique for the determination of organochlorine pesticides (OCPs) in water samples. Aqueous samples were loaded onto multiwalled carbon nanotubes as sorbent. After the elution of the desired compounds from the sorbent by using acetone, the DLLME-SFO technique was performed on the obtained solution. Variables affecting the performance of both steps such as sample solution flow rate, breakthrough volume, type and volume of the elution, type and volume of extraction solvent and salt addition were studied and optimized. The new method provided an ultra enrichment factor (8280-28221) for nine OCPs. The calibration curves were linear in the range of 0.5-1000 ng/L, and the LODs ranged from 0.1-0.39 ng/L. The RSD, for 0.01 g/L of OCPs, was in the range of 1.39-13.50% (n = 7). The recoveries of method in water samples were 70-113%.