Solvent-free method for the determination of lignin-derived phenols in sediments
| Autor: | Luiz A. S. Madureira, Mayara Pinto, Morgana Frena |
|---|---|
| Rok vydání: | 2017 |
| Předmět: |
Chromatography
Vanillin 010401 analytical chemistry Filtration and Separation 02 engineering and technology Syringic acid 021001 nanoscience & nanotechnology Solid-phase microextraction 01 natural sciences Syringaldehyde 0104 chemical sciences Analytical Chemistry Ferulic acid chemistry.chemical_compound chemistry Vanillic acid Phenols Gas chromatography 0210 nano-technology |
| Zdroj: | Journal of Separation Science. 40:2002-2008 |
| ISSN: | 1615-9306 |
| DOI: | 10.1002/jssc.201601405 |
| Popis: | A solvent-free method that uses headspace solid-phase microextraction and gas chromatography with flame ionization detection is proposed for the determination of lignin-derived phenols in sediments. The extraction and derivatization conditions for the simultaneous analysis of acetosyringone, acetovanillone, syringaldehyde, vanillin, ferulic acid, syringic acid, vanillic acid, p-hydroxybenzoic acid, and p-coumaric acid were optimized using a central composite design. After optimization, the best results were obtained with the following conditions: exposure of the polyacrylate fiber to the headspace with 60 μL of N,O-bis(trimethylsilyl)trifluoroacetamide as a derivatizing agent for 15 min and then extraction in the headspace of 100 mg of sediment (previously spiked with lignin-derived phenols) for 35 min. The accuracy of the method was estimated based on recovery tests at two concentration levels and by comparison with a high-performance liquid chromatography method reported in the literature. Based on the t-test with a confidence level of 95%, no statistical differences were observed. The detection and quantification limits for the target compounds varied according to their characteristics: values at the microgram per gram level for nonacid compounds and milligram per gram level for phenolic acids, due to the lower volatility of the derivatives. |
| Databáze: | OpenAIRE |
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