Ashraf-Khorassani M, Yang J, Rainville P, Jones M D, Fountain K J, Isaac G, Taylor L T
Department of Chemistry, Virginia Tech, Blacksburg, VA 24061, United States.
Waters Corporation, 34 Maple Street, Milford, MA 01757, United States.
J Chromatogr B Analyt Technol Biomed Life Sci. 2015 Mar 1;983-984:94-100. doi: 10.1016/j.jchromb.2014.12.012. Epub 2015 Jan 6.
Ultrahigh performance supercritical fluid chromatography (UHPSFC) in combination with sub-2μm particles and either diode array ultraviolet (UV), evaporative light scattering, (ELSD), or mass spectrometric (MS) detection has been shown to be a valuable technique for the determination of acylglycerols in soybean, corn, sesame, and tobacco seed oils. Excellent resolution on an un-endcapped single C18 column (3.0mm×150mm) with a mobile phase gradient of acetonitrile and carbon dioxide in as little as 10min served greatly as an improvement on first generation packed column SFC instrumentation. Unlike high resolution gas chromatography and high performance liquid chromatography with mass spectrometric detection, UHPSFC/MS was determined to be a superior analytical tool for both separation and detection of mono-, di-, and tri-acylglycerols as well as free glycerol itself in biodiesel without derivatization. Baseline separation of residual tri-, di-, and mono-acylglycerols alongside glycerol at 0.05% (w/w) was easily obtained employing packed column SFC. The new analytical methodology was applied to both commercial B100 biodiesel (i.e. fatty acid methyl esters) derived from vegetable oil and to an "in-house" synthetic biodiesel (i.e. fatty acid ethyl esters) derived from tobacco seed oil and ethanol both before and after purification via column chromatography on bare silica.
超高效超临界流体色谱法（UHPSFC）结合亚2μm颗粒以及二极管阵列紫外（UV）、蒸发光散射（ELSD）或质谱（MS）检测，已被证明是测定大豆油、玉米油、芝麻油和烟草籽油中酰基甘油的一种有价值的技术。在未封端的单C18柱（3.0mm×150mm）上，使用乙腈和二氧化碳的流动相梯度，在短短10分钟内即可实现出色的分离度，这极大地改进了第一代填充柱SFC仪器。与高分辨率气相色谱法和带质谱检测的高效液相色谱法不同，UHPSFC/MS被确定为一种无需衍生化即可分离和检测生物柴油中单酰基甘油、二酰基甘油、三酰基甘油以及游离甘油本身的卓越分析工具。使用填充柱SFC可轻松实现0.05%（w/w）的残留三酰基甘油、二酰基甘油和单酰基甘油与甘油的基线分离。这种新的分析方法应用于由植物油衍生的商用B100生物柴油（即脂肪酸甲酯）以及由烟草籽油和乙醇衍生的“内部”合成生物柴油（即脂肪酸乙酯），包括在通过硅胶柱色谱纯化之前和之后。
