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Solvent Exchange Module for LC-NMR Hyphenation Using Machine Vision-Controlled Droplet Evaporation

机译:使用机器视觉控制的液滴蒸发进行LC-NMR联用的溶剂交换模块

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摘要

We report the use of pendant droplet evaporation for exchange of eluents for ~1H nuclear magnetic resonance (~1H NMR) purposes. Analytes are fed and retained in 500 nL droplets, which are concentrated by evaporation and subsequently redissolved in deuterated solvent. Droplet size is monitored by machine vision (MV), and heating rates are adjusted concordingly to maintain a stable droplet volume. Evaporation control is independent of solvent properties, and the setup handles feed rates up to 7 μL min~(-1). The interface is capable of exchanging up to 90% of solvent for deuterated solvent, with a good recovery and repeatability for tomato extracts (Solanum lycopersicum). The system was capable of handling both polar and nonpolar analytes in one run. Volatiles such as formate, acetate, and lactate and the thermosensitive compound epigallocatechin gallate were recovered without significant losses. Ethanol and propionate were recovered with significant losses due to the formation of a minimum boiling azeotrope. The current setup is ideally suited for on- and off-line hyphenation of liquid chromatography and NMR, as it is comprehensive, fully automated, and easy to operate.
机译:我们报道了使用悬垂液滴蒸发来交换洗脱液,以达到〜1H核磁共振(〜1H NMR)的目的。送入分析物并保留在500 nL液滴中,将其通过蒸发浓缩,然后重新溶解在氘代溶剂中。液滴大小通过机器视觉(MV)进行监控,并一致地调节加热速率以保持稳定的液滴体积。蒸发控制与溶剂性质无关,该装置可处理最高7μLmin〜(-1)的进料速度。该界面能够将高达90%的溶剂交换为氘代溶剂,并具有良好的回收率和可重复性,可用于番茄提取物(Solanum lycopersicum)。该系统能够一次运行极性和非极性分析物。回收了挥发物,例如甲酸盐,乙酸盐和乳酸盐以及热敏化合物表没食子儿茶素没食子酸酯,没有明显损失。由于形成最小沸腾的共沸物,乙醇和丙酸酯的回收损失显着。当前设置非常全面,全自动且易于操作,非常适合液相色谱和NMR的在线和离线联用。

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