首页|Sequential combination of solid-phase sorbents to enhance the selectivity of organosulfur compounds for flavour analysis
Sequential combination of solid-phase sorbents to enhance the selectivity of organosulfur compounds for flavour analysis
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NSTL
Elsevier
? 2022 Elsevier B.V.Flavour analysis remains challenging due to the range of selectivity demands, from the extraction of multiclass volatile compounds to the purification of low-concentration odourants (e.g. organosulfur compounds) amidst the high food matrix noise. In this study, the varying selectivities of solid-phase extraction (SPE) were leveraged upon for both multiclass and organosulfur compound analysis, using coffee as a model matrix. Polymeric SPE (Bond Elut ENV) was screened for significant (p < 0.05) parameters affecting the recovery of 37 multiclass compounds, and the most influential parameters were optimised using a Box-Behnken design (elution solvent of 67:33 dichloromethane:ethyl acetate, loading pH of 4.8, and wash solvent of water). Following this, low-concentration organosulfur compounds which were challenging to detect in the complex coffee matrix were purified by adding a sequential SPE step for selectivity. A silver-based ligand-exchange SPE step (MetaSEP IC-Ag) was optimised for organosulfur compound recovery (wash solvents of dichloromethane and 43% acetonitrile in dichloromethane, elution solvent of 90 mmol/L 1,4-dithiothreitol in dichloromethane). This was found to be complementary to polymeric SPE's matrix clean-up effect (which improved average organosulfur compound recovery by 5.45 times). Finally, both multiclass and sequential organosulfur extraction techniques demonstrated good performance in terms of reproducibility (1.0–9.0%) and linearity (R2 > 0.995), allowing for the detection of 3-mercapto-3-methylbutyl formate (3.741 ± 0.387 ng/mL) in coffee samples. In conclusion, this study highlights the potential for SPE to address a variety of complex flavour analysis demands with the appropriate selection and combination of solid-phases.
NSTL
Elsevier
