Table S1. Columns used for the optimization of the HILIC × RP method used in the present research. Table S2. Identification proposed for the anthocyanins evaluated in the grape samples during ripening for a 10-week period. Figure S1. C18-RP 1DLC analysis of grape W9 (A) and wine (B). Blue: separation acquired at 280 nm; red: separation acquired at 520 nm. Figure S2. Chromatograms (280 nm) obtained for the HILIC separations obtained from a grape sample after optimization in a Zic-HILIC (A), diol (B) and silica (C) columns. Separation conditions are shown in inserts. Figure S3. Chromatograms (280 nm) obtained for the RP-based separations obtained from a grape sample after optimization in a PFP (A) and C18 (B) columns. Separation conditions are: flow rate 2 ml min-1 (Panel A) or 3 ml min-1 (panel B); elution with water (0.1% formic acid, solvent A) and acetonitrile (solvent B) as mobile phases. Specific gradients were shown in the respective chromatogram. Figure S4. 2D contour plots from the polyphenolic fraction of a grape sample (W10) obtained using different gradients and mobile phases composition in the second dimension, as indicated. Figure S5. 2D plots obtained under the optimum separation conditions for the grape samples of different ripening degree (W1 to W10).

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