Statistical optimisation applied to the spectrophotometric study of the tolmetin-Fe(III) complex.
Tolmetin sodium has been examined and determined from dosage forms as its Fe(III) complex and the method has been optimized by statistical optimization.
Adsorptive stripping voltammetric determination of the anti-inflammatory drug tolmetin in bulk form, pharmaceutical formulation and human serum
The electro-reduction of tolmetin at the hanging mercury drop electrode was studied in different supporting electrolytes using cyclic voltammetry and square-wave stripping voltammetry techniques. Voltammograms of tolmetin exhibited a single well-defined 2-electron irreversible cathodic peak in media of pH < 4, which may be attributed to reduction of the >C=O double bond of the analyte molecule. Adsorption of tolmetin onto the surface of the hanging mercury electrode was identified and each adsorbed tolmetin molecule was found to occupy an area of 0.23 nm2. A square-wave adsorptive cathodic stripping voltammetric procedure was described for the direct determination of tolmetin in bulk form and pharmaceutical formulation (Rumatol® capsules) with a limit of quantitation of 2 × 10−9 M and a mean percentage recovery of 98.35 ± 1.21% to 99.57 ± 1.23. Moreover, the described procedure was successfully applied for the direct assay of tolmetin in spiked human serum without pretreatment or extraction prior to the analysis while a quantitation limit of 5 × 10−9 M tolmetin was achieved.
Vollautomatische rechnergesteuerte Auswertung von Dünnschicht-Chromatogrammen
SummaryAutomated photometers for evaluating TLC plates by an optimized positioning of the spots in respect to the centre of the light beam are described. The evaluation can be performed by using the original measuring curve or a transformed one in respect to the Kubelka-Munk function. Two-wavelength techniques can be simulated, for the monochromator is controlled by the computer. This method has an advantage in measuring not well separated spots. In this case also an evaluation of the first derivative is often successful. The accuracy and reproducibility is given in respect to the different sources of errors: spotting, measurement, positioning and chromatography.ZusammenfassungEs werden vollautomatische DC-Photometer beschrieben, bei denen ein Rechner die optimale Positionierung der DC-Flecke im Meßspalt steuert. Es lassen sich nicht nur die normalen Meßkurven, sondern auch die gemäß der Kubelka-Munk-Funktion transformierten Kurven für die Auswertung heranziehen. Infolge der Steuerung des Wellenlängenantriebes lassen sich auch Zweiwellenlängentechniken simulieren. Für die Auswertung eignet sich auch die 1. Ableitung der Meßkurve. Die Genauigkeit und Reproduzierbarkeit wird gesondert nach Auftragefehler, Meßfehler, Positionierfehler und Fehler der Chromatographie ausgewiesen.