Ultrasound-assisted emulsification microextraction using low density solvent for analysis of toxic nitrophenols in natural waters

Abstract

An ultrasound-assisted emulsification microextraction (USAEME) based on low-density solvents was successfully applied for the extraction and pre-concentration of four toxic nitrophenols in water samples. The extracted analytes were analyzed by high-performance liquid chromatography-UV detection. The important parameters influencing the extraction efficiency were studied and optimized utilizing two different optimization methods: one variable at a time (OVAT) and central composite design (CCD). The results showed that the emulsification process can be completed in a few seconds using low-density solvents, but almost 10–20 min is necessary for high-density solvents. Under the optimum conditions (extraction solvent, 1-octanol; extraction solvent volume, 40 µL; sample pH, 3.0; salt concentration, 20% (w/v) NaCl; extraction temperature, 40 (±3)°C), limits of detection of the method were in the range of 0.25 to 1 µg L−1 and the repeatability and reproducibility of the proposed method, expressed as relative deviation, varied in the range of 2.2–4.2% and 4.7–6.9%, respectively. Linearity was found to be in the range of 1 to 200 µg L−1 and the preconcentration factors (PFs) were between 77 and 175. The relative recoveries of the four nitrophenols from water samples at spiking level of 10.0 µg L−1 were in the range of 92.0 to 115.0%.