Microchannel Thin Layer Chromatography with in situ Plate Scanning Micro-DRIFTS Detection Using Plain and Polybutadiene Modified Zirconia Stationary Phases

Thin layer chromatography (TLC) of various dyes is compared in microchannels packed with either bare zirconia (normal phase) or polybutadiene (PBD) modified zirconia (reversed phase). In situ micro-diffuse reflectance infrared Fourier transform spectroscopy (μDRIFTS) of the analyte spots is possible due to the low absorption background of both plain and PBD zirconia. An instrument coupling μDRIFTS with a motorized stage that could profile the microchannel TLC plate is developed. The retention order of anthracene and pyrene probes as a function of percent acetonitrile are generally as expected on PBD zirconia but opposite for plain zirconia. Impurities in technical grade methylene blue can be determined after TLC separation on plain zirconia. The separation and infrared identification of various dyes such as dichlorofluorescein and rhodamine B on PBD zirconia is improved using a mobile phase with an additive such as phosphate or dihexylamine that prevents band streaking.