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流动注射光致化学发光法测定水样中的抑霉唑。

Flow injection photoinduced chemiluminescence determination of imazalil in water samples.

机构信息

Integrated Coastal Management Research Institute, Higher Polytechnic School of Gandia, Polytechnic University of Valencia, Calle Paranimf 1, 46730 Grau de Gandia, Gandia, Valencia, Spain.

出版信息

Anal Bioanal Chem. 2010 Dec;398(7-8):3175-82. doi: 10.1007/s00216-010-4227-1. Epub 2010 Oct 3.

DOI:10.1007/s00216-010-4227-1
PMID:20890748
Abstract

In this work, a fast, simple and economic method is proposed for the determination of imazalil in water samples by flow injection photoinduced chemiluminescence. In this method, imazalil degrades in basic media through the use of a photoreactor, and the resulting photofragments react with ferricyanide and generate the direct chemiluminescence signal. To the authors' knowledge, this is the first time that a chemiluminescence method has been proposed for the determination of this fungicide. All physical and chemical parameters in the flow injection chemiluminescence system were optimized in the experimental setting. In the absence of preconcentration, the linear dynamic range for imazalil was 0.75-5 mg L(-1) and the detection limit was 0.171 mg L(-1). The application of solid-phase extraction with C18 cartridges allowed the elimination of interference ions, the reduction of the linear dynamic range to 15-100 μg L(-1), and a detection limit of 3.4 μg L(-1). This detection limit is below the maximum concentration level established by the Regulations of the Hydraulic Public Domain for pesticide dumping. The sample throughput after solid-phase extraction of the analyte was 12 samples h(-1). The intraday and interday coefficients of variation were below 9.9% in all cases. This method was applied to the analysis of environmental water samples, and recoveries of between 95.7 and 110% were obtained.

摘要

在这项工作中,提出了一种快速、简单和经济的方法,通过流动注射光致化学发光法测定水样中的抑霉唑。在该方法中,通过使用光反应器使抑霉唑在碱性介质中降解,得到的光碎片与铁氰化物反应并产生直接化学发光信号。据作者所知,这是首次提出用化学发光法测定这种杀菌剂。在实验设置中优化了流动注射化学发光系统中的所有物理和化学参数。在不进行预浓缩的情况下,抑霉唑的线性动态范围为 0.75-5 mg L(-1),检测限为 0.171 mg L(-1)。采用 C18 小柱固相萃取,可以消除干扰离子,将线性动态范围降低到 15-100 μg L(-1),检测限为 3.4 μg L(-1)。这个检测限低于水利公共领域农药倾倒规定中规定的最大浓度水平。在分析物的固相萃取后,样品的吞吐量为 12 个样品 h(-1)。在所有情况下,日内和日间变异系数均低于 9.9%。该方法应用于环境水样的分析,回收率在 95.7%至 110%之间。

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