A technique for creating devices for ultrathin layer chromatography (UTLC) using an electrospinning method is described. The devices use a nanofibrous stationary phase with fiber diameters that are 400 run. Separations of mixtures of laser dyes and mixtures of steroidal compounds were performed to illustrate the capabilities of these new UTLC media. The complete analyses were found to require very little development time and require less solvent than typical TU methods. The efficiency of the separations was substantially improved compared to that determined using commercial phases. The retention properties and efficiency of the technique are discussed as are the effects of mat thickness and mobile phase composition on the chromatographic properties of the devices.