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采用多元优化双分散液液微萃取-GC-MS 法同时测定湖水和废水中的异菌脲、菌核净和氯氟菌唑。

Simultaneous determination of iprodione, procymidone, and chlorflurenol in lake water and wastewater matrices by GC-MS after multivariate optimization of binary dispersive liquid-liquid microextraction.

机构信息

Department of Environmental Engineer, Institute of Science, Bülent Ecevit University, 67100, Zonguldak, Turkey.

Faculty of Art and Science, Department of Chemistry, Yıldız Technical University, 34210, Istanbul, Turkey.

出版信息

Environ Monit Assess. 2018 Sep 25;190(10):607. doi: 10.1007/s10661-018-6961-3.

DOI:10.1007/s10661-018-6961-3
PMID:30255206
Abstract

This study reports the optimization of a binary dispersive liquid-liquid microextraction method for the determination of iprodione, procymidone, and chlorflurenol by gas chromatography mass spectrometry. The study was aimed at using two extraction solvents to increase the extraction efficiency of all analytes. The binary solvents recorded results higher than the mono-solvents. After examining the effects of main experimental parameters and their interactions by analysis of variance, 200 μL of binary mixture (dichloromethane and 1,2-dichloroethane), 2.5 mL of ethanol, and 15 s vortex were obtained as optimum parameters. The detection and quantification limits calculated for the analytes were found to be between 0.30-1.6 and 1.0-5.3 ng/mL, respectively. Enhancement in detection power calculated as a ratio of the binary extraction detection limit to the detection limit of direct GC-MS analysis was 105-, 214-, and 233-fold for chlorflurenol, iprodione, and procymidone, respectively. In order to check the accuracy of the developed method, recovery study was performed. Water sampled from a lake and two wastewater samples from treatment facilities were spiked at two concentrations, and the percent recovery calculated for the samples ranged between 87 and 116%. These results confirmed the suitability of the method to real samples for accurate determination of the analytes at trace levels.

摘要

本研究报告了一种二元分散液相微萃取方法的优化,用于气相色谱质谱法测定异丙菌胺、菌核净和氯氟醇。该研究旨在使用两种萃取溶剂来提高所有分析物的萃取效率。二元溶剂的记录结果高于单溶剂。通过方差分析考察了主要实验参数及其相互作用的影响后,得到了 200μL 二元混合物(二氯甲烷和 1,2-二氯乙烷)、2.5mL 乙醇和 15s 涡旋作为最佳参数。计算得出的分析物检测限和定量限分别为 0.30-1.6 和 1.0-5.3ng/mL。以二元萃取检测限与直接 GC-MS 分析检测限的比值计算得出的检测能力增强倍数分别为氯氟醇、异丙菌胺和菌核净的 105、214 和 233 倍。为了检查所开发方法的准确性,进行了回收率研究。在两个处理设施的废水样品中,分别在两个浓度下对取自湖泊的水样进行了加标,计算出的样品回收率在 87%至 116%之间。这些结果证实了该方法适用于真实样品,可在痕量水平准确测定分析物。

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