Comparison of ASE and SFE with Soxhlet, Sonication, and Methanolic Saponification Extractions for the Determination of Organic Micropollutants in Marine Particulate Matter

Abstract

The methods of accelerated solvent extraction (ASE) and supercritical fluid extraction (SFE) of polycyclic aromatic hydrocarbons (PAHs), aliphatic hydrocarbons, and chlorinated hydrocarbons from marine samples were investigated. The results of extractions of a certified sediment and four samples of suspended particulate matter (SPM) were compared to classical Soxhlet (SOX), ultrasonication (USE), and methanolic saponification extraction (MSE) methods. The recovery data, including precision and systematic deviations of each method, were evaluated statistically. It was found that recoveries and precision of ASE and SFE compared well with the other methods investigated. Using SFE, the average recoveries of PAHs in three different samples ranged from 96 to 105%, for ASE the recoveries were in the range of 97−108% compared to the reference methods. Compared to the certified values of sediment HS-6, the average recoveries of SFE and ASE were 87 and 88%, most compounds being within the limits of confidence. Also, for alkanes the average recoveries by SFE and ASE were equal to the results obtained by SOX, USE, and MSE. In the case of SFE, the recoveries were in the range 93−115%, and ASE achieved recoveries of 94−107% as compared to the other methods. For ASE and SFE, the influence of water on the extraction efficiency was examined. While the natural water content of the SPM sample (56 wt %) led to insufficient recoveries in ASE and SFE, quantitative extractions were achieved in SFE after addition of anhydrous sodium sulfate to the sample. Finally, ASE was applied to SPM-loaded filter candles whereby a mixture of n-hexane/acetone as extraction solvent allowed the simultaneous determination of PAHs, alkanes, and chlorinated hydrocarbons.