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一种新型液相微萃取-气相色谱-火焰光度检测法用于水样中有机磷农药的萃取与测定

Extraction and determination of organophosphorus pesticides in water samples by a new liquid phase microextraction-gas chromatography-flame photometric detection.

作者信息

Khalili-Zanjani Mohammad Reza, Yamini Yadollah, Yazdanfar Najmeh, Shariati Shahab

机构信息

Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, P.O. Box 14115-175, Tehran, Iran.

出版信息

Anal Chim Acta. 2008 Jan 14;606(2):202-8. doi: 10.1016/j.aca.2007.11.032. Epub 2007 Nov 23.

Abstract

A rapid, sensitive and efficient liquid phase microextraction (LPME) method was developed to determine trace concentrations of some organophosphorus pesticides in water samples. This method combines liquid phase microextraction with gas chromatographic (GC) analysis in a simple and inexpensive apparatus involving very little organic solvent consumption. It involves exposing a floated drop of an organic solvent on the surface of aqueous solution in a sealed vial. Experimental parameters which control the performance of LPME such as type of organic solvent, organic solvent and sample volumes, sample stirring rate, sample solution temperature, salt addition and exposure time were investigated and optimized. Finally, the enrichment factor, dynamic linear range (DLR), limit of detection (LOD) and precision of the method were evaluated by the water samples spiked with organophosphorus pesticides. Using optimum extraction conditions, very low detection limits (0.01-0.04mugL(-1)) and good linearities (0.9983<r(2)<0.9999) were achieved. The LPME was performed for determination of organophosphorus pesticides in different types of natural water samples and acceptable recoveries (96-104%) and precisions (3.5<R.S.D.%<8.9) were obtained. The results suggested that the newly proposed LPME method is a rapid, accurate and effective sample preparation method and could be successfully applied for extraction and determination of organophosphorus pesticides in water samples.

摘要

开发了一种快速、灵敏且高效的液相微萃取(LPME)方法,用于测定水样中痕量浓度的某些有机磷农药。该方法将液相微萃取与气相色谱(GC)分析相结合,采用一种简单且成本低廉的装置,有机溶剂消耗量极少。它包括在密封小瓶中的水溶液表面暴露一滴漂浮的有机溶剂。研究并优化了控制LPME性能的实验参数,如有机溶剂类型、有机溶剂和样品体积、样品搅拌速率、样品溶液温度、加盐量和暴露时间。最后,通过添加有机磷农药的水样评估了该方法的富集因子、动态线性范围(DLR)、检测限(LOD)和精密度。在最佳萃取条件下,实现了极低的检测限(0.01 - 0.04μg L⁻¹)和良好的线性关系(0.9983 < r² < 0.9999)。对不同类型的天然水样进行LPME测定有机磷农药,获得了可接受的回收率(96 - 104%)和精密度(3.5 < R.S.D.% < 8.9)。结果表明,新提出的LPME方法是一种快速、准确且有效的样品制备方法,可成功应用于水样中有机磷农药的萃取和测定。

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