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Cloud point extraction coupled with ultrasonic-assisted back-extraction for the determination of organophosphorus pesticides in concentrated fruit juice by gas chromatography with flame photometric detection

机译:浊点萃取-超声辅助反萃取-气相色谱-火焰光度检测法测定浓缩果汁中有机磷农药

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摘要

A new method for the determination of nine organophosphorus pesticides (OPPs): Dichlorvos, metham-idophos, acephate, diazinon, dimethoate, chlorpyrifos, parathion-methyl, malathion and parathion-ethyl in concentrated fruit juice was developed using the cloud point extraction coupled with ultrasonic-assisted back-extraction prior to gas chromatography with flame photometric detection (GC-FPD) analysts. The parameters and variables that affect the extraction were investigated. Under optimum conditions: a solution containing 6% (W/V) polyethylene glycol 6000 (PEG 6000) and 20% (W/V) Na_2SO_4 for the extraction of the OPPs. The coacervation phase obtained was back extracted with ethyl acetate. The upper ethyl acetate solution was centrifugated simply for further cleanup for the sake of automatic injection. A preconcentration factor of 50 was obtained for these nine pesticides. Using this method, the limits of detection (LOD)and limits of quantification (LOQ) were in the range of 0.5-3.0 and 1.5-9.0 μg kg~(-1) in concentrated fruit juice, respectively; the relative standard deviations (RSD) were <9%.
机译:浊点萃取结合浊点萃取技术开发了一种测定九种有机磷农药的新方法:敌敌畏,甲胺磷,乙酰甲胺,二嗪农,乐果,毒死rif,对硫磷甲基,马拉硫磷和对硫磷乙基超声辅助反萃取,然后进行气相色谱和火焰光度检测(GC-FPD)分析人员。研究了影响提取的参数和变量。在最佳条件下:用于提取OPP的溶液,其中包含6%(W / V)的聚乙二醇6000(PEG 6000)和20%(W / V)的Na_2SO_4。将获得的凝聚相用乙酸乙酯反萃取。为了自动进样,将上层乙酸乙酯溶液简单地离心以进一步纯化。这九种农药的预浓缩系数为50。使用该方法,浓缩果汁中的检出限(LOD)和定量限(LOQ)分别为0.5-3.0和1.5-9.0μgkg〜(-1)。相对标准偏差(RSD)小于9%。

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