Simultaneous determination of diclofenac and its common counter-ions in less than 1 minute using capillary electrophoresis with contactless conductivity detection.

This paper presents a method for fast and simultaneous determination of diclofenac (DCF) and its common counter-ions (potassium, sodium, and diethylammonium) using CE with capacitively coupled contactless conductivity detection (CE-C(4) D). On the basis of a single electropherogram (about 50 s), the proposed method allows the determination of the stoichiometry, absolute quantification and evaluation of the degradation degree of the active pharmaceutical ingredient (DCF). A linear working range from 100 to 500 µmol/L was obtained for all analytes in an equimolar TRIS/TAPS (10 mmol/L) solution as the background electrolyte as well as adequate LOD (7, 6, 7, and 10 µmol/L for K(+) , Na(+) , diethylammonium, and DCF, respectively). The proposed method was applied to the analysis of pharmaceutical formulations (tablets and spray form) with similar results to those achieved by HPLC (DCF) or flame photometry (K and Na) at a 95% confidence level.

Direct amperometric determination of tert-butylhydroquinone in biodiesel.

The direct amperometric determination of tert-butylhydroquinone (TBHQ) in biodiesel at an unmodified glassy carbon electrode is reported. A biodiesel aliquot was added into an electrochemical cell containing a 75% (v/v) ethanol-water solution under stirring (with final concentration of 50 mmol L(-1) HClO(4)). The amperometric method involved the continuous application of three sequential potential pulses to the working electrode (700 mV for 300 ms, 0 mV for 100 ms and -50 mV for 1s). TBHQ was continuously monitored at the first (direct oxidation) and optionally at the second (reduction) potential pulse while the third potential pulse was applied for cleaning of the electrode surface. For comparison, the samples were also analyzed by high-performance liquid-chromatography and a good agreement between the results was verified. Recovery values for spiked samples were between 90% and 95% and the reproducibility of the proposed method was around 5% (n=5). The proposed method can be easily adapted for on-site analysis.