Quantitative determination of Piroxicam by TLC–MALDI TOF MS

A quantitative thin-layer chromatography (TLC)–matrix-assisted laser desorption (MALDI) TOF mass spectrometry (MS) method for the determination of Piroxicam has been developed. Following preliminary experiments three different approaches to the incorporation of the internal standard (Tenoxicam) into the TLC plates were investigated. These were: (a) adding the internal standard to the mobile phase and pre-developing the plate, (b) coating the plate with internal standard by electrospraying prior to matrix application and finally, (c) mixing the internal standard into the matrix solution and electrospraying both. The most successful method was that where the internal standard was pre-developed over the plate. For this method linearity was observed over the range between 400 and 800 ng of Piroxicam. The precision was found to be in the range of 1–9% R.S.D. from the average detected value (<F>n=5</F>), dependent on the amount of analyte on the TLC plate. The proposed method was accurate with ±2% deviation from the known amount of Piroxicam in the sample spot. [Copyright &y& Elsevier]