Development of a pressurized liquid extraction and clean-up procedure for the determination of alpha-endosulfan, beta-endosulfan and endosulfan sulfate in aged contaminated Ethiopian soils

Pressurized liquid extraction (PLE) was investigated for the extraction of two endosulfan isomers and their metabolite from two real contaminated soil samples. PLE for 3 x 10 min at 100 degrees C was proven to be more exhaustive than Soxhlet extraction (SOX) in one soil sample. On the other soil sample investigated the method was found to be equally exhaustive as SOX. The use of hazardous organic solvents such as n-hexane, toluene, and diethyl ether has been avoided in PLE and clean-up. Instead less toxic solvents have been used both at the extraction step (acetone/n-heptane) and clean-up step (ethyl acetate/n-heptane). A column Florisil clean-up procedure that consumes relatively low solvent volumes has been optimized and applied to purify soil extracts. The developed analytical procedure was validated by applying it to a certified reference soil material (CRM811-050). A recovery of 103% total endosulfan residue was obtained versus certified values. (c) 2005 Elsevier B.V. All rights reserved.