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The Use of Silver Solid Amalgam Electrodes for Voltammetric and Amperometric Determination of Nitrated Polyaromatic Compounds Used as Markers of Incomplete Combustion

机译:固态银汞齐电极用于伏安法和安培法测定硝化多芳族化合物(不完全燃烧的标记物)的用途

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摘要

Genotoxic nitrated polycyclic aromatic hydrocarbons (NPAHs) are formed during incomplete combustion processes by reaction of polycyclic aromatic hydrocarbons (PAHs) with atmospheric nitrogen oxides. 1-Nitropyrene, 2-nitrofluorene, and 3-nitrofluoranthene as the dominating substances are used as markers of NPAHs formation by these processes. In the presented study, voltammetric properties and quantification of these compounds and of 5-nitroquinoline (as a representative of environmentally important genotoxic heterocyclic compounds) have been investigated using a mercury meniscus modified silver solid amalgam electrode (m-AgSAE), which represent a nontoxic alternative to traditional mercury electrodes. Linear calibration curves over three orders of magnitude and limits of determination mostly in the 10−7 mol L−1 concentration range were obtained using direct current and differential pulse voltammetry. Further, satisfactory HPLC separation of studied analytes in fifteen minutes was achieved using 0.01 mol L−1 phosphate buffer, pH 7.0 : methanol (15 : 85, v/v) mobile phase, and C18 reversed stationary phase. Limits of detection of around 1 · 10−5 mol L−1 were achieved using amperometric detection at m-AgSAE in wall-jet arrangement for all studied analytes. Practical applicability of this technique was demonstrated on the determination of 1-nitropyrene, 2-nitrofluorene, 3-nitrofluoranthene, and 5-nitroquinoline in drinking water after their preliminary separation and preconcentration using solid phase extraction with the limits of detection around 1 · 10−6 mol L−1.
机译:遗传毒性硝化多环芳烃(NPAH)是在不完全燃烧过程中通过多环芳烃(PAH)与大气氮氧化物的反应形成的。作为主要物质的1-硝基trop,2-硝基芴和3-硝基荧蒽被用作通过这些方法形成NPAH的标志。在本研究中,使用汞弯月形修饰的银固体汞齐电极(m-AgSAE)研究了这些化合物和5-硝基喹啉(作为对环境重要的遗传毒性杂环化合物的代表)的伏安特性和定量替代传统的汞电极。使用直流电和差分脉冲伏安法获得了三个数量级的线性校准曲线,其测定极限主要在10 −7 mol L -1 浓度范围内。此外,使用0.01 mol L -1 磷酸盐缓冲液,pH 7.0:甲醇(15:85,v / v)流动相和C18反相固定相在15分钟内完成了满意的HPLC分析物分离。使用m-AgSAE的安捷伦检测技术在壁式喷射装置中对所有研究的分析物均达到了约1·10 −5 mol L −1 的检测限。使用固相萃取对饮用水中的1-硝基py,2-硝基芴,3-硝基荧蒽和5-硝基喹啉进行初步分离和预浓缩后,其检测极限约为1·10 <1,从而证明了该技术的实用性。 sup> -6 mol L -1

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