Ashraf-Khorassani M, Yan Q, Akin A, Riley F, Aurigemma C, Taylor L T
Department of Chemistry, Virginia Tech, Blacksburg, VA 24061-0212, United States.
Global Research & Development, Pfizer Inc., Groton, CT 06340, United States.
J Chromatogr A. 2015 Oct 30;1418:210-217. doi: 10.1016/j.chroma.2015.09.025. Epub 2015 Sep 10.
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.
正相快速液相色谱法的方法开发传统上采用在裸硅胶上使用常规溶剂的薄层色谱（TLC）进行初步筛选。本文报道了通过TLC迁移结果与常规极性/非极性液体混合物的相关性，以及通过在裸硅胶上使用一系列二氧化碳流动相改性剂进行梯度洗脱的填充柱超临界流体色谱（SFC）保留时间，将其扩展到绿色快速色谱法。本文针对8种三元混合物中的24种中性分析物分别描述了TLC/SFC相关性的可行性。TLC/SFC相关性的实验标准假定如下：在三种分离的混合物组分中，SFC/UV/MS保留时间（tR）增加；而在相同的分离混合物组分中，TLC迁移率（Rf）降低。对于大多数测试的极性有机溶剂，观察到TLC与SFC的成功相关性，以甲醇作为CO2改性剂在裸硅胶上进行SFC以及以甲醇/二氯甲烷混合物在裸硅胶上进行TLC时观察到最佳结果。
