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oai:uvadoc.uva.es:10324/737372026-01-13T21:00:43Zcom_10324_1134com_10324_931com_10324_894col_10324_1213
UVaDOC author Mateo Vivaracho, Laura María author Cacho, Juan author Ferreira, Vicente 2025-01-13T12:18:05Z 2025-01-13T12:18:05Z 2008 Journal of Chromatography A, 1185 (2008) 9–18 0021-9673 https://uvadoc.uva.es/handle/10324/73737 10.1016/j.chroma.2008.01.037 9 1 18 Journal of Chromatography A 1185 A fast method for the determination of aroma-powerful polyfunctional thiols at ng L−1 level has been developed. Mercaptans are selectively retained in a 50 mg solid-phase extraction cartridge and derivatization takes place in the same cartridge at room temperature (25 °C) in 20 min by adding small amounts of pentafluorobenzyl bromide (PFBBr) and a strong alkali: 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU). The corresponding derivatives are further eluted and determined by gas chromatography–negative ion mass spectrometry (GC–NCI-MS). Isolation, derivatization, clean-up, elution and calibration conditions were examined. Carrying the reaction in the cartridge makes it possible to use water and non-polar reagents simultaneously, to avoid large volumes of toxic solvent, and to eliminate the excess of reagent. This was last accomplished by the reaction with mercaptoglycerol and further rinsing with a hydromethanolic solution. The method makes it possible to simultaneously determine 2-methyl-3-furanthiol (MF), 2-furfurylthiol (2-furanmethanethiol) (FFT), 4-mercapto-4-methyl-2-pentanone (MP) (as its methoxime), 3-mercaptohexylacetate (MHA) and 3-mercaptohexanol (MH). Absolute limits of detection were 0.2 (MF), 0.1 (FFT), 0.1 (MP), 0.3 (MHA) and 2 (MH) ng L−1. Repeatability (1% < RSD < 20%) and linearity (0.978 < R2 < 0.999) were satisfactory. Problems with matrix effects were solved by the use of deuterated analogues for MP, MHA and MH and by avoiding the oxidation of analytes and standards via addition of cysteine and EDTA. The different aspects of the method optimization are discussed. eng Attribution-NonCommercial-NoDerivatives 4.0 Internacional Improved solid-phase extraction procedure for the isolation and in-sorbent pentafluorobenzyl alkylation of polyfunctional mercaptans info:eu-repo/semantics/article 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URL https://uvadoc.uva.es/bitstream/10324/73737/1/1-s2.0-S0021967308001258-main.pdf File MD5 0b047e7057ea9aab2f0574c3dcbd4c57 1232419 application/pdf 1-s2.0-S0021967308001258-main.pdf