期刊
TALANTA
卷 99, 期 -, 页码 972-983出版社
ELSEVIER
DOI: 10.1016/j.talanta.2012.07.073
关键词
Ionic liquids; Ionic liquid-based surfactants; Organic contaminants; Sediment samples; Focused microwave-assisted extraction; In situ preconcentration; High-performance liquid chromatography
资金
- Structuring Project in Marine Sciences (EXMAR) from the Canary Agency for Research and Innovation (ACIISI)
- Spanish ministry of Innovation and Science (MICINN)
- University of La Laguna (ULL)
- MICINN [CTQ2008-06253/BQU]
- Analytical and Surface Chemistry Program in the Division of Chemistry and the Separation and Purification Process Program in the Chemical, Environmental, Bioengineering, and Transport Systems Division from the National Science Foundation for a CAREER grant [CHE-0748612]
- Division Of Chemistry
- Direct For Mathematical & Physical Scien [0748612] Funding Source: National Science Foundation
The determination of a group of organic contaminants from marine sediments samples including three polycyclic aromatic hydrocarbons, five alkylphenols (i.e., bisphenol-A or nonylphenol) and one paraben has been carried out using an extraction/preconcentration strategy with ionic liquid-based surfactants and high-performance liquid chromatography (HPLC) with diode array detection (DAD). Sediments are first extracted using two IL-based surfactants, specifically 1-hexadecyl-3-methyl imidazolium bromide (C(16)MIm-Br) and 1-hexadecyl-3-butyl imidazolium bromide (C(16)C(4)Im-Br), as the extraction media in a microwave-assisted extraction (MAE) procedure, followed by a novel in situ preconcentration method. The optimized MAE method requires 0.1 g of sediment and 5 mL of 40 mM C(16)MIm-Br IL solution. The extracts are then centrifuged and filtered. The subsequent preconcentration in situ approach consists of the insolubilization of an IL-based surfactant formed by a metathesis reaction using the anion-exchange reagent lithium bis[(trifluoromethane)sulfonyl]imide (LiNTf2), which produces an analyte enriched IL microdroplet. The optimized in situ approach utilizes 4 mL of the filtered extract, which are mixed with acetonitrile and 92 mu L of LiNTf2 solution (0.5 g mL(-1)), heated, vortexed and centrifuged. The formed IL microdroplet is then simply diluted with acetonitrile (similar to 100 mu L) and injected in the chromatograph without any further clean-up steps. The overall extraction/preconcentration method requires approximately 25 min in spite of dealing with complex solid samples, is nearly free of organic solvent (requires similar to 900 mu L of acetonitrile per sample), and produces high preconcentration factors and quantification limits down to 0.04 mg kg(-1) using HPLC-DAD. (C) 2012 Elsevier B.V. All rights reserved.
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