Most research on the extraction of high-priced compounds from vineyard/wine byproducts has traditionally been focused on grape seeds and skins as raw materials. Vine-shoots can represent an additional source to those materials, the characteristics of which could depend on the cultivar. A comparative study of hydroalcoholic extracts from 18 different vineyard cultivars obtained by superheated liquid extraction (SHLE), microwave-assisted extraction (MAE), and ultrasound-assisted extraction (USAE) is here presented. The optimal working conditions for each type of extraction have been investigated by using multivariate experimental designs to maximize the yield of total phenolic compounds, measured by the Folin-Ciocalteu method, and control hydroxymethylfurfural because of the organoleptic properties of furanic derivatives and toxicity at given levels. The best values found for the influential variables on each extraction method were 80% (v/v) aqueous ethanol at pH 3, 180 °C, and 60 min for SHLE; 140 W and 5 min microwave irradiation for MAE; and 280 W, 50% duty cycle, and 7.5 min extraction for USAE. SHLE reported better extraction efficiencies as compared to the other two approaches, supporting the utility of SHLE for scaling-up the process. The extracts were dried in a rotary evaporator, reconstituted in 5 mL of methanol, and finally subjected to liquid-liquid extraction with n-hexane to remove nonpolar compounds that could complicate chromatographic separation. The methanolic fractions were analyzed by both LC-DAD and LC-TOF/MS, and the differences in composition according to the extraction conditions were studied. Compounds usually present in commercial wood extracts (mainly benzoic and hydroxycinnamic acids and aldehydes) were detected in vine-shoot extracts.
A study of the nonvolatile fraction of extracts from vine shoots obtained by superheated ethanol-water mixtures is presented. The influence of the temperature, extraction time, and percentage of ethanol on extraction was investigated by a multivariate experimental design to maximize the yield of total phenolic compounds, measured by using the Folin-Ciocalteu method. The best values found for these variables were 80% (v/v) ethanol, 240 degrees C, and 60 min. Under these conditions, the effect of pH was also investigated, and a strong improvement of yield was observed by decreasing the pH. The extracts were subject to liquid-liquid extraction with n-hexane. The remaining polar phase was dried in a rotary evaporator and then reconstituted in 10 mL of water. The insoluble residue was dissolved in 10 mL of methanol. Both fractions (aqueous and methanolic) were analyzed by HPLC, and the differences in composition according to the extraction conditions were studied. Compounds usually present in commercial wood extracts were identified (mainly benzoic and hydroxycinnamic acids and aldehydes); the most abundant were quantified, and the stability of the identified phenolic families under different extraction conditions was also investigated. Finally, the superiority of the superheated liquid extraction over conventional solid-liquid extraction was demonstrated.
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