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Microwave‐assisted extraction combined with dispersive liquid–liquid microextraction as a new approach to determination of chlorophenols in soil and sediments
Author(s) -
Naeeni Mohammad Hosein,
Yamini Yadollah,
Rezaee Mohammad,
Seidi Shahram
Publication year - 2012
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201100978
Subject(s) - extraction (chemistry) , chromatography , disperser , chemistry , detection limit , chlorobenzene , solvent , liquid–liquid extraction , acetone , sample preparation , analytical chemistry (journal) , materials science , biochemistry , organic chemistry , composite material , catalysis
A new method was applied for extraction of five chlorophenols from soil and marine sediment samples. Microwave‐assisted extraction coupled with dispersive liquid–liquid microextraction followed by semi‐automated in‐syringe back‐extraction technique was used as an extraction technique. Microwave‐assisted extraction was performed by using 2.0 m L of alkaline water at p H 10.0. After extraction, the p H of extraction solution was adjusted at 6.0 and dispersive liquid–liquid microextraction procedure was done using 1.0 m L of acetone as a disperser solvent and 37.0 μ L of chlorobenzene as extraction solvent. About 20.0 ± 0.5 μ L sedimented phase was collected after centrifugation step. Then, chlorophenols were back extracted into 20 μ L of alkaline water at p H 12.0 within the microsyringe. Finally, 20.0 μ L of aqueous solution was injected into high performance liquid chromatography with ultra violet detection for analysis. The obtained recovery and preconcentration factors for the analytes were in the range of 68.0–82.0% and 25–30, respectively, with relative standard deviations ≤7.6%. The limits of the detection were found in the range of 0.0005–0.002 mg/kg. The method provides a simple and fast procedure for the extraction and determination of chlorophenols in soil and marine sediment samples.