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A New Approach for Voltammetric Determination of Nefopam and its Metabolite
Electroanalysis ( IF 2.7 ) Pub Date : 2019-12-09 , DOI: 10.1002/elan.201900595 Liliya Dubenska 1 , Olha Dushna 1 , Solomiya Pysarevska 2 , Mykola Blazheyevskiy 3
Electroanalysis ( IF 2.7 ) Pub Date : 2019-12-09 , DOI: 10.1002/elan.201900595 Liliya Dubenska 1 , Olha Dushna 1 , Solomiya Pysarevska 2 , Mykola Blazheyevskiy 3
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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.
中文翻译：
伏安法测定奈福opa及其代谢产物的新方法
在本文中，我们描述了测定奈福opa生物碱及其代谢产物-N-氧化物的一种新的简单伏安法。在滴下的汞电极（DME）和固态银汞合金电极（AgSAE）上，奈福opa的N-氧化物减少，可有效替代汞和化学修饰的电极。还原包括两个单电子阶段，每个阶段伴随一个质子转移。可以通过用过氧一硫酸钾氧化从奈福opa物质中获得奈福opa的N-氧化物。研究了各种因素对N氧化物定量收率（pH，氧化持续时间，试剂浓度）以及DME和p-AgSAE上N氧化物减少的影响（pH，背景电解质的性质，电势和累积时间）。结果表明，随着镇痛剂浓度的增加，还原电流呈线性增加。定量限为10DME时为-6 mol L -1，p-AgSAE时为10 -7 mol L -1。所开发的方法用于分析注射用“ Nefopam”的商业药物溶液，回收率为96.7％，以及加标的人尿液样品。相对标准偏差低于5％时，可实现出色的重复性。
更新日期：2019-12-09
中文翻译：
伏安法测定奈福opa及其代谢产物的新方法
在本文中，我们描述了测定奈福opa生物碱及其代谢产物-N-氧化物的一种新的简单伏安法。在滴下的汞电极（DME）和固态银汞合金电极（AgSAE）上，奈福opa的N-氧化物减少，可有效替代汞和化学修饰的电极。还原包括两个单电子阶段，每个阶段伴随一个质子转移。可以通过用过氧一硫酸钾氧化从奈福opa物质中获得奈福opa的N-氧化物。研究了各种因素对N氧化物定量收率（pH，氧化持续时间，试剂浓度）以及DME和p-AgSAE上N氧化物减少的影响（pH，背景电解质的性质，电势和累积时间）。结果表明，随着镇痛剂浓度的增加，还原电流呈线性增加。定量限为10DME时为-6 mol L -1，p-AgSAE时为10 -7 mol L -1。所开发的方法用于分析注射用“ Nefopam”的商业药物溶液，回收率为96.7％，以及加标的人尿液样品。相对标准偏差低于5％时，可实现出色的重复性。
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