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Determination of organophosphorous pesticides in wastewater samples using binary-solvent liquid-phase microextraction and solid-phase microextraction:A comparative study

机译:二元溶剂液相微萃取和固相微萃取测定废水样品中的有机磷农药:比较研究

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摘要

A simple and efficient binary solvent-based two-phase hollow fiber membrane (HFM)-protected liquid-phase microextraction (BN-LPME) technique for moderately polar compounds was developed.Six organophosphorous pesticides (OPPs) (triethylphosphoroth-ioate,thionazin,sulfotep,phorate,disulfoton,methyl parathion and ethyl parathion) were used as model compounds and extracted from 10-mL wastewater with a binary-solvent (toluenerhexane,1:1) mixture.Some important extraction parameters,such as extraction time,effect of salt,sample pH and solvent ratio composition were optimized.BN-LPME combined with gas chromatography/mass spectrometric (GC/MS) analysis provided repeatability (R.S.D.s < 12%,n = 4),and linearity (r < 0.994) and solid-phase microextraction provides comparable of R.S.D.S < 13%,n = 4 and linearity (r = <0.966) for spiked water samples.The limits of detection (LODs) were in the range of 0.3-11.4 ng L~(-1) for BN-LPME and 3.1-120.5 ng L~(-1) for SPME at (S/N = 3) under GC/MS selective ion monitoring mode.In addition to high enrichment,BN-LPME also served as a sample cleanup procedure,with the HFM act as a filtering medium to prevent large particles and extraneous materials from being extracted.To investigate and compare their applicability,the BN-LPME and SPME procedures were applied to the detection of OPPs in domestic wastewater samples.
机译:开发了一种简单有效的基于二元溶剂的两相中空纤维膜(HFM)保护的液相微萃取(BN-LPME)技术,用于中等极性化合物的制备。六种有机磷农药(OPP)(碘化三乙基磷酸酯,噻嗪,硫杂磷) ,磷酸酯,二硫代芬,甲基对硫磷和乙基对硫磷)作为模型化合物,用二元溶剂(甲苯己烷,1:1)混合物从10mL废水中提取。一些重要的提取参数,例如提取时间,盐的影响BN-LPME与气相色谱/质谱(GC / MS)分析相结合可提供重复性(RSDs <12%,n = 4),线性(r <0.994)和固相微萃取对加标水样的RSDS <13%,n = 4和线性(r = <0.966)具有可比性.BN-的检出限(LODs)在0.3-11.4 ng L〜(-1)范围内。在GC / MS选择下,在(S / N = 3)下SPME的LPME和3.1-120.5 ng L〜(-1) BN-LPME除了高富集外,还用作样品净化程序,以HFM作为过滤介质,以防止大颗粒和外来物质被提取出来。要研究和比较它们的适用性,BN -LPME和SPME程序用于检测生活废水样品中的OPP。

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