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3D amperometry in the liquid chromatographic determination of trace pharmaceutical and herbicide emerging compounds

机译:液相色谱中的3D安培法测定痕量药物和除草剂新化合物

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In this work, we innovatively applied the 3D amperometry detection, coupled to liquid chromatography, for the determination of a mixture of chromatographically unresolved compounds (two herbicides-monuron and bentazon, one drug-propranolol and the main metabolite of an antiepileptic drug-5-(4MODIFIER LETTER PRIME-hydroxyphenyl)-5-phenylhydantoin). Exploiting the post-chromatographic current integration, a scanning waveform was successfully applied to explore a wide range of potentials (0.0-1.3 V) to find the peculiar oxidative potential value for each compound. This approach allowed us to obtain 3D chromatograms (elution time vs potential vs current) in which coeluted species could be clearly distinguished. Quantitation was easily obtained by extraction of 2D chromatograms (elution time vs integrated current), from the 3D ones, at the optimised waveform time ranges (800-1,000 msec and 1,500-1,700 msec, corresponding to 0.6-0.8 V and 1.0-1.2, respectively). Validation of the proposed 3D amperometry method was performed in terms of linearity, limits of detection and quantitation and repeatability. Matrix effect was studied by statistical treatment on a wastewater effluent. By coupling an on-line solid phase extraction step prior to separation and detection by 3D amperometry, detection limits were significantly reduced (57 ng/L for bentazon, with recovery yields of 82.9 +/- 10.9%). It is worth mentioning that this value fully satisfies the requirements of the 98/83/CE directive for the determination of bentazon in groundwater.
机译:在这项工作中,我们创新地将3D安培法检测与液相色谱联用,用于确定色谱中未分离的化合物(两种除草剂-莫努隆和苯达松,一种药物-普萘洛尔和抗癫痫药5的主要代谢物)的混合物。 (4修饰字母PRIME-羟基苯基)-5-苯基乙内酰脲)。利用色谱后电流积分,成功地应用了扫描波形来探索各种电位(0.0-1.3 V),以找到每种化合物的特殊氧化电位值。这种方法使我们能够获得3D色谱图(洗脱时间vs电位vs电流),在其中可以清楚地区分共洗脱物。在优化的波形时间范围(800-1,000毫秒和1,500-1,700毫秒,分别对应于0.6-0.8 V和1.0-1.2)下,从3D色谱图中提取2D色谱图(洗脱时间与积分电流),即可轻松获得定量结果。分别)。在线性,检测和定量限以及可重复性方面对提出的3D安培法进行了验证。通过对废水进行统计处理研究了基质效应。通过在分离和通过3D安培法检测之前耦合在线固相萃取步骤,可大大降低检测限(苯达松的检测限为57 ng / L,回收率为82.9 +/- 10.9%)。值得一提的是,该值完全满足98/83 / CE指令中测定地下水中苯达松的要求。

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