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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Analysis of hexachlorocyclohexanes in aquatic samples by one-step microwave-assisted headspace control led-temperature liquid-phase microextraction and gas chromatography with electron capture detection
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Analysis of hexachlorocyclohexanes in aquatic samples by one-step microwave-assisted headspace control led-temperature liquid-phase microextraction and gas chromatography with electron capture detection

机译:一步微波辅助顶空控制的LED液相微萃取-气相色谱-电子捕获检测分析水中的六氯环己烷

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摘要

A microwave-assisted headspace controlled-temperature liquid-phase microextraction (HS-CT-LPME) technique was applied for the one-step sample extraction of hexachlorocyclohexanes (HCHs) from aqueous samples with complicate matrices, followed by gas chromatographic (CC) analysis with electron capture detector (ECD) Microwave heating was applied to accelerate the evaporation of HCHs into the headspace and an external-cooling system was used to control the temperature in the sampling zone for HS-LPME Parameters affecting extraction efficiency, such as LPME solvent. sampling position and temperature, microwave power and irradiation time (the same as sampling time), sample pH. and salt addition were thoroughly investigated From experimental results, the following conditions were selected for the extraction of HCHs from 10-mL water sample(pH 2.0) by Using I-octanol as the LPME solvent. with sampling done at 38 degrees C for 6 min under 167 W of microwave irradiation The detections were linear in the concentration of 1-10 mu/L for alpha-HCH and gamma-HCH, and 1-100 mu g/L for beta-HCH and delta-HCH Detection limits were 0 05. 0.4. 0 03 and 0. 1 mu/L for alpha-, beta-, gamma- and delta-HCH, respectively Environmental water samples were analyzed with recovery between 86 4% and 102 4% for farm-field water, and between 92.2% and 98.6% for river water. The proposed method proved to serve as a simple, rapid, sensitive, inexpensive, and eco-friendly procedure for the determination of HCHs in aqueous samples.
机译:微波辅助顶空控制温度液相微萃取(HS-CT-LPME)技术用于从具有复杂基质的水性样品中一步提取六氯环己烷(HCH),然后通过气相色谱(CC)分析电子捕获检测器(ECD)进行微波加热以加速六氯环己烷向顶空的蒸发,并使用外部冷却系统控制影响萃取效率的HS-LPME参数(例如LPME溶剂)的采样区温度。采样位置和温度,微波功率和辐照时间(与采样时间相同),样品pH值。从实验结果出发,选择了以下条件,以1-辛醇为LPME溶剂从10毫升水样品(pH 2.0)中提取六氯环己烷。在167 W微波辐照下于38摄氏度下进行6分钟采样。α-六氯环己烷和γ-六氯环己烷的检测浓度呈线性,线性为1-10μg/ L,β-六氯环己烷的检测浓度为1-100μg/ L。六氯环己烷和增量六氯环己烷的检出限为0 05. 0.4。分别为0、03和0. 1 mu / L,用于六氯环己烷,β,γ和δ六氯环己烷的分析结果表明,农田水的回收率在86 4%和102 4%之间,而回收率在92.2%和102%之间。河流水为98.6%。实践证明,该方法可作为一种简单,快速,灵敏,廉价且环保的方法来测定水性样品中的六氯环己烷。

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