作者: Rosa Perestrelo , Catarina L. Silva , José S. Câmara
DOI: 10.1016/J.CHROMA.2015.01.020
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摘要: Abstract An improved, reliable and powerful analytical strategy based on digitally controlled microextraction by packed sorbent (MEPS) combined with ultrahigh pressure liquid chromatography (UHPLC) was validated for the simultaneous identification quantification of major furanic derivatives, namely 5-hydroxymethyl-2-furaldehyde (5HMF), 5-methyl-2-furaldehyde (5MF), 2-furaldehyde (2F) 2-furyl methyl ketone (2FMK), in fortified wines. To enhance extraction efficiency target derivates, several influencing parameters, such as number loading cycles, nature elution solvent volume, were evaluated optimized. In addition ability different MEPS materials, C2, C8, C18, SIL, M1, R-AX, R-CX PGC, also tested. The optimal conditions involved 3 × 200 μL wine samples through a C8 syringe placed semi-automatic eVolH followed using 200 μL MeOH:H2O (95:5, v/v). derivates separation achieved CORTECS UPLC® C18 column an ultrafast chromatographic run (within 4 min). method performance assessed dry/medium dry (D/MD) sweet/medium sweet (S/MS) model wines terms selectivity, linearity, limit detection (LOD), quantitation (LOQ), accuracy, precision matrix effect, matrix-matched calibration. Good linearity obtained regression coefficient (r2) higher than 0.992. A good attained (RSD MEPSC8/UHPLC–PDA successfully applied to analyze 26 Madeira from types (D/MD, S/MS) ages. results revealed suitable tool which combines sensitivity, effectiveness, reduced analysis time simple procedure. Principal component (PCA) suggested that can be organized their age PC1, are mainly characterized 5HMF.