title: Ultrahigh performance supercritical fluid chromatography of lipophilic compounds with application to synthetic and commercial biodiesel.
abstract: 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.
authors: Department of Chemistry, Virginia Tech, Blacksburg, VA 24061, United States.
authors: M
authors: M
authors: Ashraf-Khorassani
authors: Waters Corporation, 34 Maple Street, Milford, MA 01757, United States.
authors: J
authors: J
authors: Yang
authors: Waters Corporation, 34 Maple Street, Milford, MA 01757, United States.
authors: P
authors: P
authors: Rainville
authors: Waters Corporation, 34 Maple Street, Milford, MA 01757, United States.
authors: M D
authors: MD
authors: Jones
authors: Waters Corporation, 34 Maple Street, Milford, MA 01757, United States.
authors: K J
authors: KJ
authors: Fountain
authors: Waters Corporation, 34 Maple Street, Milford, MA 01757, United States.
authors: G
authors: G
authors: Isaac
authors: Department of Chemistry, Virginia Tech, Blacksburg, VA 24061, United States. Electronic address: ltaylor@vt.edu.
authors: L T
authors: LT
authors: Taylor
mesh_terms: D056804:Biofuels / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D025924:Chromatography, Supercritical Fluid / Q000379:methods*; D005240:Feasibility Studies; D005990:Glycerol / Q000032:analysis; D007267:Injections; D008055:Lipids / Q000737:chemistry*; D013058:Mass Spectrometry; D012542:Scattering, Radiation; D014280:Triglycerides / Q000032:analysis; D014466:Ultraviolet Rays
chemical_list: D056804:Biofuels; D008055:Lipids; D014280:Triglycerides; D005990:Glycerol
keywords: Biodiesel purity test; Evaporative light scattering detection; Normal phase chromatography; Octa-decyl bonded silica particles; Tobacco seed oil; Ultrahigh performance supercritical fluid chromatography