In present paper we described a new simple voltammetric method of determination of nefopam alkaloid and its metabolite – N‐oxide. N‐oxide of nefopam is reduced at the dropping mercury electrode (DME) and silver solid amalgam electrodes (AgSAE), which can effectively replace mercury and chemically modified electrodes. The reduction consists of two one‐electron stages each accompanied with one proton transfer. N‐oxide of nefopam can be obtained from nefopam substance by oxidation with potassium peroxymonosulfate. It was studied the effect of various factors on N‐oxide quantitative yield (pH, oxidation duration, reagents concentration) as well as on the reduction of N‐oxide at DME and p‐AgSAE (pH, the nature of background electrolyte, potential and time of accumulation). It was showed that the reduction current linearly increased with increasing of concentration of analgesic. Limit of quantiation is 10−6 mol L−1 at DME and 10−7 mol L−1 at p‐AgSAE. The developed method was applied for the analysis of commercial drug solution for injection “Nefopam” with recovery of 96.7 %, as well as for the spiked human urine samples. Excellent repeatability with a relative standard deviation below 5 % was achieved.

In the present paper, for the first time, the electrochemical behaviour of nicotine metabolite nicotine N-oxide (NNO) on static mercury dropping electrode (SMDE) and mercury meniscus modified silver solid amalgam electrode (m-AgSAE) has been reported. Nicotine N-oxide is reduced forming one peak at the potential -0.78 V on SDME and -0.86 V on m-AgSAE in Britton-Robinson buffer medium at pH 4.5 using cyclic voltammetry (CV). One electron and one proton take part in the reaction of NNO reduction. Calibration graphs for NNO determination using linear sweep voltammetry (LSV) on SDME and square-wave voltammetry (SWV) and differential pulse voltammetry (DPV) on m-AgSAE were obtained. Limit of detection (LOD) is 0.13 μM on SDME, and 0.16 μM (SWV) and 0.29 μM (DPV) on m-AgSAE. Since NNO can be used as an analytical form for nicotine voltammetric determination, so the developed methods were applied for the analysis of pharmaceutical preparations, and the recoveries from 97.3 to 104.6 % were achieved. Also, the elaborated methods were used in the analysis of biological fluids, and tobacco products. The obtained results were compared to those indicated in the certificates of drugs analysis, and to the results, obtained by reference methods (HPLC and GC).

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