HPTLC, with UV and MS detection, and preparative-layer chromatography for analysis and purification of synthesis products

Abstract

A high-performance thin-layer chromatographic (HPTLC) method with UV detection has been established for evaluation of the purity of synthesis products. Purity measured by HPTLC-UV and LC-UV was in good agreement, confirming the suitability of the method for this application. Atmospheric-pressure matrix-assisted laser desorption/ionization mass spectrometry (AP-MALDI-MS) was used to confirm and identify the product zones on the plate before purification by preparative-layer chromatography (PLC). AP-MALDI-MS was more selective than UV detection and was an easy and rapid means of identification of synthesis products in situ on the plate. A new and simple device for isolation of PLC-separated product zones is described. With PLC and the new isolation device, synthesis products in sub-milligram amounts were successfully purified.