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Detection of triazole pesticides in environmental water and juice samples using dispersive liquid-liquid microextraction with solidified sedimentary ionic liquids

机译:固相沉淀离子液体分散液-液微萃取技术检测环境水和果汁样品中的三唑类农药

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摘要

A novel in situ metathesis reaction combined with an ultrasound-assisted dispersive liquid-liquid microextraction based on the solidification of sedimentary ionic liquids (in situ UA-SSIL-DLLME) was combined with high-performance liquid chromatography (HPLC) to detect four triazole pesticides in water and juice samples. In this method, the hydrophobic ionic liquid [P-4448][PF6], formed in situ by the hydrophilic ionic liquid [P-4448]Br and the anion-exchange reagent KPF6, was used as the microextraction solvent. The extraction procedure was assisted by ultrasound at 50 W for 5 min. After centrifugation and cooling, [P-4448][PF6] was sedimented at the bottom and easily collected by decanting the aqueous phase directly. Various parameters affecting the extraction efficiency, such as the quantity of [P-4448]Br, the molar ratio of [P-4448]Br to KPF6, salt addition, ultrasound time, centrifugation rate and time, and sample pH, were evaluated. Good linearities with correlation coefficients greater than 0.99 were obtained under the optimum conditions. The limits of detection varied between 0.90 and 1.38 mu g L-1, and the enrichment factors were in the range of 94-101. The recoveries of these four triazole pesticides ranged from 85.18% to 91.14%, with relative standard deviations less than 4.86% and 5.87% for intra-day (n = 3) and inter-day (n = 3), respectively. The proposed method was then successfully applied to analyze the target compounds in environmental water and juice samples.
机译:基于沉淀离子液体凝固的超声原位复分解反应与超声辅助分散液-液微萃取(原位UA-SSIL-DLLME)结合高效液相色谱法(HPLC)相结合,检测出四种三唑类农药在水和果汁样品中。在该方法中,将由亲水性离子液体[P-4448] Br和阴离子交换试剂KPF6原位形成的疏水性离子液体[P-4448] [PF6]用作微萃取溶剂。超声提取程序在50 W下超声5分钟。离心并冷却后,[P-4448] [PF6]沉淀在底部,可通过直接倾析水相轻松收集。评价了影响萃取效率的各种参数,例如[P-4448] Br的量,[P-4448] Br与KPF6的摩尔比,加盐,超声时间,离心率和时间以及样品pH值。在最佳条件下获得了良好的线性,相关系数大于0.99。检测限在0.90和1.38μg L-1之间变化,富集因子在94-101范围内。这四种三唑类农药的回收率在日内(n = 3)和日间(n = 3)的相对标准偏差分别小于4.86%和5.87%。该方法成功地用于分析环境水和果汁样品中的目标化合物。

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