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Ion-pair assisted liquid–liquid extraction for selective separation and analysis of multiclass pesticide residues in environmental waters

机译:离子对辅助液液萃取,用于环境水中多种农药残留的选择性分离和分析

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A new ion-pair assisted liquida€“liquid extraction (IPA-LLE) method in combination with high performance liquid chromatography-diode array detection (HPLC-DAD) has been proposed for the determination of ten multiclass (six sulfonylurea and four organophosphorus ) pesticides in environmental waters. In the IPA-LLE procedure, the ion-pairing reagent tetrabutylammonium hydrogen sulfate and the organic solvent, acetonitrile, were used for extraction of the target analytes. Various parameters influencing the extraction efficiency such as the type, composition and volume of the ion-pair, volume of acetonitrile, sample pH, type and composition of the salt and effect of sonication time were studied and optimal conditions were established. Under the optimum conditions, the limits of detection and quantification of the proposed method were in the ranges of 0.5a€“3.0 ??g La?’1 and 1.8a€“10.0 ??g La?’1, respectively, and calibration curves were linear within the range of 1.8a€“450 ??g La?’1, with coefficients of determination of 0.993 or better. Intra- and inter-day precision studies, expressed as relative standard deviations, at three concentration levels, were in the range of 0.4a€“9.4%. The relative recoveries of the spiked environmental water samples were in the range of 73a€“105%, except for nicosulfuron in lake water. The results of the study revealed that the developed method involves efficient sample preparation allowing the preconcentration of analytes, followed by the use of HPLC-DAD for quantitative analysis.
机译:提出了一种结合高效液相色谱-二极管阵列检测(HPLC-DAD)的离子对辅助液体萃取(IPA-LLE)新方法,用于测定十种多类(六种磺酰脲类和四种有机磷)农药在环境水域中。在IPA-LLE方法中,使用离子配对试剂硫酸氢四丁铵和有机溶剂乙腈提取目标分析物。研究了影响萃取效率的各种参数,例如离子对的类型,组成和体积,乙腈的体积,样品的pH,盐的类型和组成以及超声处理时间的影响,并确定了最佳条件。在最佳条件下,所提出方法的检出限和定量限分别在0.5a·3.0g·La·1和1.8a·10.0g·g·La1·1之间。曲线在1.8a?450 ?? g La?'1的范围内是线性的,测定系数为0.993或更高。日内和日间精密度研究在三个浓度水平上用相对标准偏差表示,范围为0.4a%至9.4%。除了湖水中的烟嘧磺隆外,加标环境水样品的相对回收率在73%至105%之间。研究结果表明,开发的方法涉及有效的样品制备,允许对分析物进行预浓缩,然后使用HPLC-DAD进行定量分析。

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