Meloxicam (MLC), 4-hydroxy-2-methyl-N-(5-methyl-2-thiazolyl)-2H-1,2-benzo thiazine-3-carboxamide-1,1-dioxide, is a highly potent non-steroidal anti-inflammatory drug (NSAID) of the enolic acid class of oxicam derivatives. 1,2) This drug is indicated for the treatment of rheumatoid arthritis, osteoarthritis, and other joint diseases.2) Due to the vital importance of MLC determination in pharmaceutical preparations and in biological fluids, many analytical techniques have been reported in literature. MLC has been determined in pharmaceutical preparations using spectroscopic, [3][4][5][6][7] HPLC [8][9][10][11][12][13] and electrochemical [14][15][16][17][18] methods. Studies of the therapeutic and toxic effects of drugs require a sensitive method for determination of them at a trace level. All reported spectroscopic methods suffer from low sensitivity. On the other hand, high performance liquid chromatographic methods, while having the advantage of requiring minimal sample preparation, are relatively slow and expensive, require filtration, degassing and expensive grades of reagents, eluents and equipment. In addition, the most of the reported electrochemical methods are based on the reduction of MLC on dropping or hanging mercury electrodes. Radi et al. have developed an electrochemical oxidation method for determination of MLC in tablet dosage form using a carbon paste electrode.16) According to this report, MLC is irreversibly oxidized from amide and enol functions over pH range 2-11.5 in buffer media. Adsorptive stripping voltammetry has been demonstrated as a sensitive analytical method for a wide range of pharmaceutical compounds adsorbing on the electrode surface.19) As a result, a wide variety of substances possessing surface-active properties are easily measurable at very low concentration levels.20) The adsorptive properties of a glassy carbon electrode can be changed with the electrochemical pretreatment procedure. Electrode surface modifications and pretreatments have been widely used to improve the electrochemical responses of biological compounds and to construct electrochemical detectors for liquid chromatography involving the detection of analytes that oxidize only at extreme positive potentials. [21][22][23] The behavior of carbon electrodes at high positive potentials has received considerable interest owing to a desire to improve both the activity and reproducibility of carbon electrodes. The objective of the present work was to develop an adsorptive stripping voltammetric procedure for the determination of MLC, with higher sensitivity than the reported ones. It has been found that MLC could be adsorbed on an electrochemically pretreated glassy carbon electrode (EPGCE). Using this phenomenon and by accumulating this compound at the electrode surface prior to a differential pulse voltammetry and linear sweep voltammetry measurements, a higher sensitivity has been readily achieved. This work deals with the application of the proposed voltammetric methods to assay MLC in biological samples and pharm...