Optimization by factorial design of focused microwave assisted extraction of polycyclic aromatic hydrocarbons from marine sediment

Abstract

The Focused Microwave (FMW) assisted extraction for organic contaminant analysis, such as polycyclic aromatic hydrocarbons (PAHs), in environmental matrices, was studied and optimized using a factorial design. The effects and interactions of five parameters on the extraction recovery were investigated in a few experiments with a good accuracy: irradiation power and time, volume and nature of solvent, and percentage of moisture of the matrix. The results show that the percentage of water added to the freeze-dried matrix can significantly increase the extraction recovery. The irradiation power has also a positive effect. The choice of solvent is significant: a mixture of heptane/ethanol (80/20, v/v) allows better results than dichloromethane. Some interactions between percentage of moisture and the two previous parameters have been demonstrated: the effect of power and nature of solvent depends on the water content. Some optimal conditions have been established: 10 mL of heptane/ethanol (80/20, v/v), extraction time of 2 min, and different possible pairs of moisture content and irradiation power (140 W and 0% of moisture or 20 W and 40% of moisture) according to the need and wish of the experimentalist; or 10 mL of dichloromethane, extraction time of 2 min, 20 W and 40% of moisture. These optimized conditions provide very good recoveries compared to conventional extraction such as Soxhlet (near 100%) for the model matrix (a marine sediment) used for the factorial design. FMW extraction is a good alternative to Soxhlet extraction with reduction of time and reduction of solvent volume. This study shows that it is possible to substitute chlorinated solvent by a less toxic solvent, like a mixture of heptane and ethanol.