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分散液液微萃取结合反相高效液相色谱法在环境水样中两种杀菌剂测定中的应用

Application of dispersive liquid-liquid microextraction and reversed phase-high performance liquid chromatography for the determination of two fungicides in environmental water samples.

作者信息

Cheng Jing, Zhou Yiwen, Zuo Mei, Dai Liping, Guo Xiaojie

机构信息

Key Laboratory of Pesticide & Chemical Biology, Ministry of Education, College of Chemistry, Central China Normal University, Wuhan, 430079, China.

出版信息

Int J Environ Anal Chem. 2010 Sep 15;90(11):845-855. doi: 10.1080/03067310903180468. Epub 2010 Aug 11.

Abstract

Dispersive liquid-liquid microextraction (DLLME) has been developed for the extraction and preconcentration of diethofencarb (DF) and pyrimethanil (PM) in environmental water. In the method, a suitable mixture of extraction solvent (50 μL carbon tetrachloride) and dispersive solvent (0.75 mL acetonitrile) are injected into the aqueous samples (5.00 mL) and the cloudy solution is observed. After centrifugation, the enriched analytes in the sediment phase were determined by HPLC-VWD. Different influencing factors, such as the kind and volume of extraction and dispersive solvent, extraction time and salt effect were investigated. Under the optimum conditions, the enrichment factors for DF and PM were both 108 and the limit of detection were 0.021 ng mL(-1) and 0.015ng mL(-1), respectively. The linear ranges were 0.08-400ng mL(-1) for DF and 0.04-200ng mL(-1) for PM. The relative standard deviation (RSDs) were both almost at 6.0% (n = 6). The relative recoveries from samples of environmental water were from the range of 87.0 to 107.2%. Compared with other methods, DLLME is a very simple, rapid, sensitive (low limit of detection) and economical (only 5 mL volume of sample) method.

摘要

已开发出分散液液微萃取(DLLME)法用于环境水中乙霉威(DF)和嘧霉胺(PM)的萃取和预浓缩。该方法是将萃取溶剂(50 μL四氯化碳)和分散溶剂(0.75 mL乙腈)的合适混合物注入水样(5.00 mL)中,观察到溶液变浑浊。离心后,通过高效液相色谱-可变波长检测器(HPLC-VWD)测定沉淀相中富集的分析物。研究了不同影响因素,如萃取溶剂和分散溶剂的种类及体积、萃取时间和盐效应。在最佳条件下,DF和PM的富集因子均为108,检测限分别为0.021 ng mL⁻¹和0.015 ng mL⁻¹。DF的线性范围为0.08 - 400 ng mL⁻¹,PM的线性范围为0.04 - 200 ng mL⁻¹。相对标准偏差(RSDs)均几乎为6.0%(n = 6)。环境水样的相对回收率在87.0%至107.2%范围内。与其他方法相比,DLLME是一种非常简单、快速、灵敏(检测限低)且经济(仅需5 mL样品体积)的方法。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/1f9a/2936117/f36c19838bdd/geac4_465_f1.jpg

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