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用于气相色谱-火焰光度检测之前环境水样中有机磷农药测定的均相液-液微萃取法

Homogeneous Liquid-Liquid Microextraction for Determination of Organophosphorus Pesticides in Environmental Water Samples Prior to Gas Chromatography-Flame Photometric Detection.

作者信息

Berijani Sana, Sadigh Mirhanif, Pournamdari Elham

机构信息

Department of Applied Chemistry, Faculty of Science, Islamic Azad University, South Tehran Branch, Tehran, Iran

Department of Civil Engineering, University of Science and Culture, Tehran, Iran.

出版信息

J Chromatogr Sci. 2016 Jul;54(6):1061-7. doi: 10.1093/chromsci/bmw020. Epub 2016 Mar 3.

DOI:10.1093/chromsci/bmw020
PMID:26944949
Abstract

In this study, homogeneous liquid-liquid microextraction (HLLME) was developed for preconcentration and extraction of 15 organophosphorus pesticides (OPPs) from water samples coupling with gas chromatography followed by a flame photometric detector (HLLME-GC-FPD). In this method, OPPs were extracted by the homogeneous phase in a ternary solvent system (water/acetic acid/chloroform). The homogeneous solution was excluded by the addition of sodium hydroxide as a phase separator reagent and a cloudy solution was formed. After centrifugation (3 min at 5,000 rpm), the fine particles of extraction solvent (chloroform) were sedimented at the bottom of the conical test tube (10.0 ± 0.5 µL). Furthermore, 0.5 µL of the sedimented phase was injected into the GC for separation and determination of OPPs. Optimal results were obtained under the following conditions: volume of the extracting solvent (chloroform), 53 µL; volume of the consolute solvent (acetic acid), 0.76 mL and concentration of sodium hydroxide, 40% (w/v). Under the optimum conditions, the enrichment factors of (260-665), the extraction percent of 75.8-104%, the dynamic linear range of 0.03-300 µg L(-1) and the limits of detection of 0.004-0.03 µg L(-1) were obtained for the OPPs. This method was successfully applied for the extraction and determination of the OPPs in environmental water samples.

摘要

在本研究中,开发了均相液-液微萃取(HLLME)方法,用于对水样中的15种有机磷农药(OPPs)进行预浓缩和萃取,并与气相色谱-火焰光度检测器联用(HLLME-GC-FPD)。在该方法中,OPPs在三元溶剂体系(水/乙酸/氯仿)的均相中被萃取。通过加入氢氧化钠作为相分离试剂来排除均相溶液,从而形成浑浊溶液。离心(5000转/分钟,3分钟)后,萃取溶剂(氯仿)的细颗粒沉淀在锥形试管底部(10.0±0.5微升)。此外,将0.5微升沉淀相注入气相色谱仪中,用于OPPs的分离和测定。在以下条件下获得了最佳结果:萃取溶剂(氯仿)体积为53微升;共溶剂(乙酸)体积为0.76毫升;氢氧化钠浓度为40%(w/v)。在最佳条件下,OPPs的富集因子为260-665,萃取率为75.8-104%,动态线性范围为0.03-300微克/升,检测限为0.004-0.03微克/升。该方法成功应用于环境水样中OPPs的萃取和测定。

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