Department of Analytical Chemistry, Annex Marie Curie Building, Campus of Rabanales, University of Córdoba, Córdoba, Spain.
J Agric Food Chem. 2012 Mar 28;60(12):3051-60. doi: 10.1021/jf205078k. Epub 2012 Mar 12.
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.
大多数从葡萄园/葡萄酒副产物中提取高价化合物的研究传统上都集中在葡萄种子和果皮作为原料。葡萄枝梢可以作为这些材料的另一种来源,其特性可能取决于品种。本文比较了超临界液体萃取(SHLE)、微波辅助萃取(MAE)和超声辅助萃取(USAE)从 18 种不同葡萄园品种中获得的水醇提取物。通过多元实验设计研究了每种提取方法的最佳工作条件,以最大限度地提高总酚化合物的产量,用福林-肖卡法测定,控制羟甲基糠醛,因为呋喃衍生物的感官特性和在给定水平下的毒性。每种提取方法的变量的最佳值为 80%(v/v)pH3 的水乙醇,180°C,60 分钟为 SHLE;140W 和 5 分钟微波辐射为 MAE;280W、50%占空比和 7.5 分钟提取为 USAE。与其他两种方法相比,SHLE 的提取效率更高,支持 SHLE 用于放大过程。提取物在旋转蒸发器中干燥,在 5ml 甲醇中重新配制,最后用正己烷进行液液萃取以去除可能使色谱分离复杂化的非极性化合物。用 LC-DAD 和 LC-TOF/MS 分析甲醇馏分,并根据提取条件研究了成分的差异。在葡萄枝梢提取物中检测到了通常存在于商业木材提取物中的化合物(主要是苯甲酸和羟基肉桂酸及其醛)。