title: Feasibility of correlating separation of ternary mixtures of neutral analytes via thin layer chromatography with supercritical fluid chromatography in support of green flash separations.
abstract: Method development for normal phase flash liquid chromatography traditionally employs preliminary screening using thin layer chromatography (TLC) with conventional solvents on bare silica. Extension to green flash chromatography via correlation of TLC migration results, with conventional polar/nonpolar liquid mixtures, and packed column supercritical fluid chromatography (SFC) retention times, via gradient elution on bare silica with a suite of carbon dioxide mobile phase modifiers, is reported. Feasibility of TLC/SFC correlation is individually described for eight ternary mixtures for a total of 24 neutral analytes. The experimental criteria for TLC/SFC correlation was assumed to be as follows: SFC/UV/MS retention (tR) increases among each of the three resolved mixture components; while, TLC migration (Rf) decreases among the same resolved mixture components. Successful correlation of TLC to SFC was observed for most of the polar organic solvents tested, with the best results observed via SFC on bare silica with methanol as the CO2 modifier and TLC on bare silica with a methanol/dichloromethane mixture.
authors.affiliation: Department of Chemistry, Virginia Tech, Blacksburg, VA 24061-0212, United States.
authors.forename: M
authors.initials: M
authors.lastname: Ashraf-Khorassani
authors.affiliation: Global Research & Development, Pfizer Inc., Groton, CT 06340, United States.
authors.forename: Q
authors.initials: Q
authors.lastname: Yan
authors.affiliation: Global Research & Development, Pfizer Inc., Groton, CT 06340, United States.
authors.forename: A
authors.initials: A
authors.lastname: Akin
authors.affiliation: Global Research & Development, Pfizer Inc., Groton, CT 06340, United States.
authors.forename: F
authors.initials: F
authors.lastname: Riley
authors.affiliation: Pfizer, Inc., Worldwide Medicinal Chemistry, La Jolla Laboratories, San Diego, CA 92121, United States.
authors.forename: C
authors.initials: C
authors.lastname: Aurigemma
authors.affiliation: Department of Chemistry, Virginia Tech, Blacksburg, VA 24061-0212, United States. Electronic address: ltaylor@vt.edu.
authors.forename: L T
authors.initials: LT
authors.lastname: Taylor
mesh_terms: D002245:Carbon Dioxide / Q000737:chemistry; D002853:Chromatography, Liquid; D025924:Chromatography, Supercritical Fluid / Q000379:methods*; D002855:Chromatography, Thin Layer / Q000379:methods*; D005240:Feasibility Studies; D000432:Methanol / Q000737:chemistry; D009930:Organic Chemicals / Q000032:analysis*; D012822:Silicon Dioxide / Q000737:chemistry; D012997:Solvents / Q000737:chemistry
chemical_list: D009930:Organic Chemicals; D012997:Solvents; D002245:Carbon Dioxide; D012822:Silicon Dioxide; D000432:Methanol
keywords: Correlation; Modifiers; Neutral analytes; SFC/MS retention; Supercritical fluid chromatography; TLC migration; Thin layer chromatography