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超临界流体从葡萄渣中连续提取高附加值分子
2024/08/22 11:13
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方案摘要：
产品配置单：
SFE LAB100ml超临界二氧化碳萃取系统
型号： SFE LAB100
产地： 法国
品牌： 法国SFE
¥100万 - 150万
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Abstract
Inspired by the concept of organic waste valorisation and heading towards a sustainable economy, a green chemistry extraction technique involving supercritical carbon dioxide (SC-CO2) along with water as a co-solvent was employed for the main winery by-product (grape pomaces). The objective was to selectively extract high-value added molecules, in particular phenolic compounds and polysaccharides. The experimental design involved applying three distinct temperature conditions (40, 60, and 80 °C), and a constant pressure of 400 bar. Phenolic compounds and high-molecular weight isolates (449–478 kDa) containing low methoxyl (% DE = 23) pectic substances were detected in the SC-CO2 extracts accompanied by water as a co-solvent. The phenolic acids, namely, gallic (GA), protocatechuic (PCA), coumaric (CouA), and caftaric (CTA), and flavonoids, namely, procyanidin B1 (PRC B1), procyanidin B2 (+) (PRC B2), (+) catechin (CT), and (−) epicatechin (ECT) were found in all the extracts under the tested experimental conditions. The following study underscores the potential of the pressurized CO2/H2O medium as an effective solvent with minimal environmental impacts for the comprehensive valorisation of the main winery by-product, specifically targeting polysaccharides and phenolic compounds.
受有机废物价值化概念的启发，并朝着可持续经济的方向发展，一种涉及超临界二氧化碳（SC-CO2）和水作为共溶剂的绿色化学提取技术被用于酿酒厂的主要副产品（葡萄渣）。目的是选择性地提取高附加值的分子，特别是酚类化合物和多糖。实验设计涉及应用三种不同的温度条件（40、60和80°C）和400bar的恒压。在SC-CO2提取物中检测到含有低甲氧基（%DE=23）果胶物质的酚类化合物和高分子量分离物（449-478 kDa），并伴有水作为共溶剂。在测试的实验条件下，所有提取物中都发现了酚酸，即没食子酸（GA）、原儿茶酸（PCA）、香豆酸（CouA）和咖啡酸（CTA），以及黄酮类化合物，即原花青素B1（PRC B1）、原花青素B2（+）（PRC B2）、儿茶素（CT）和表儿茶素（ECT）。以下研究强调了加压CO2/H2O介质作为一种有效溶剂的潜力，该溶剂对环境的影响最小，可全面稳定主要酒厂副产品，特别是针对多糖和酚类化合物。
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2. Materials and methods
2.1. Materials
The grape pomace was obtained from a white grape variety (Marsannay Aligoté) from Côte de Nuits vineyard, France and stored at −20 °C in the plastic thermo bags. The wet grape pomace had a moisture content of 73.2%.The standards of white wine-related phenolic compounds such as gallic, protocatechuic, hydroxybenzoic, caftaric, gentisic, caffeic, coumaric, and chlorogenic acids and hydroxytyrosol, tyrosol, procyanidin B1, B2, (+) catechin and (−) epicatechin were purchased from Sigma-Aldrich (Steinheim, Germany). The monosaccharide standards (mannitol, L-fucose, L-rhamnose, L-arabinose, D-galactose, D-glucose, D-mannose, D-xylose, D-galacturonic and glucuronic acids) were purchased from Acros Organics and Sigma-Aldrich. Sodium hydroxide (NaOH) solution 46/48% (Fisher Bioblock), sodium acetate (NaOAc) (Sigma-Aldrish), trifluoroacetic acid (TFA) (Merck) and all the above-mentioned chemicals were of analytical grade.
2.2. Sample pre-treatment
Prior to extraction, the grape pomace was subjected to pre-treatment steps involving oven-drying at 50 °C followed by grinding using an industrial grinder (SK 100, RETSCH®). The powder was passed through 1 mm mesh. The exact particle size distribution within the powder was determined using a laboratory sieve shaker and the size variation of particles was 50% of 200 μm, 40% under 400–500 μm and the remaining 10% less <1 mm which included larger particles mainly from the grape seeds. The powder was stored in thermo bags at −20 °C until further use.2.3. Supercritical CO2 extraction on grape pomaces
The supercritical SC-CO2 machine (SFE process, Nancy, France) coupled with two pumps, main CO2 and co-solvent, with a maximum pressure capacity of 1000 bar was used in this study. The instrument is equipped with an extraction basket (stainless steel) with a capacity of 100 mL and an autoclave cylinder, which directs the extracts to the back pressure regulator (BPR) (Fig. 1). The cooling system was filled with glycerol and the CO2 flow was recycled in the system. The observation of the extracts was possible thanks to the transparent sapphire separator. Various temperature sensors were placed in the system monitoring important temperature changes within the system.本研究中使用了超临界SC-CO2机器（SFE process, Nancy, France），该机器配有两个泵，主CO2泵和共溶剂泵，最大压力容量为1000bar。该仪器配备了一个容量为100毫升的提取器（不锈钢）和一个高压釜，将提取物引导到背压调节器（BPR）（图1）。冷却系统充满甘油，CO2流在系统中循环。得益于透明的蓝宝石隔膜，可以观察到提取物。系统中放置了各种温度传感器，用于监测系统内的重要温度变化。
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