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分散液液微萃取与高效液相色谱联用富集快速测定环境水样中苯甲酰脲类农药。

Dispersive liquid-phase microextraction in combination with HPLC for the enrichment and rapid determination of benzoylurea pesticides in environmental water samples.

机构信息

Beijing Key Laboratory of Oil and Gas pollution Control, College of Geosciences, China University of Petroleum, Beijing, China.

出版信息

J Sep Sci. 2013 Jul;36(14):2323-9. doi: 10.1002/jssc.201300138. Epub 2013 Jun 10.

Abstract

Benzoylurea (BU) insecticides have contributed greatly to the output of crops. Their residue in the environment put serious threats on human health and environmental safety. In this study, we have established a new, rapid, and reliable method for the monitoring of typical BU insecticides such as diflubenzuron, flufenoxuron, triflumuron, and chlorfluazuron with dispersive liquid-liquid microextraction prior to HPLC. Chlorobenzene and ethanol were employed as the extraction solvent and disperser solvent, respectively. The possible parameters which would influence the extraction efficiency such as the kinds and volumes of extraction and disperser solvents, extraction time, sample pH, centrifuging time, and salting-out effect were optimized in detail. Under the optimal conditions, the linear range of proposed method was in the range of 1.0-70 μg/L. The detection limits varied from 0.24 to 0.82 μg/L and the precision of the method was <6.5% (RSD, n = 6). The proposed method was validated with real water samples and satisfactory spiked recoveries were achieved. All these results indicate that the proposed method is a low cost, easy to operate, efficient, and sensitive method for the analysis of BU insecticides in water samples.

摘要

苯甲酰脲(BU)类杀虫剂对作物产量有很大的贡献。它们在环境中的残留对人类健康和环境安全构成了严重威胁。在本研究中,我们建立了一种新的、快速和可靠的方法,用于在 HPLC 之前通过分散液-液微萃取监测典型的 BU 类杀虫剂,如除虫脲、氟铃脲、伏虫隆和氟虫脲。氯苯和乙醇分别用作萃取溶剂和分散溶剂。详细优化了可能影响萃取效率的参数,如萃取和分散溶剂的种类和体积、萃取时间、样品 pH 值、离心时间和盐析效应。在最佳条件下,该方法的线性范围为 1.0-70 μg/L。检测限为 0.24-0.82 μg/L,方法的精密度<6.5%(RSD,n=6)。该方法已用水样进行验证,获得了令人满意的加标回收率。所有这些结果表明,该方法是一种低成本、易于操作、高效灵敏的方法,可用于水样中 BU 类杀虫剂的分析。

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