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分散液液微萃取结合气相色谱-微电子捕获检测(GC-µECD)用于测定水样中有机氯农药的评估。

Evaluation of dispersive liquid-liquid microextraction coupled with gas chromatography-microelectron capture detection (GC-µECD) for the determination of organochlorine pesticides in water samples.

作者信息

Zhao Zhonghua, Zhang Lu, Wu Jinglu, Jin Miao, Fan Chengxin

机构信息

State Key Laboratory for Lake Science and Environment Research, Nanjing Institute of Geography and Limnology, Chinese Academy of Sciences, Nanjing, China.

出版信息

Anal Sci. 2011;27(5):547. doi: 10.2116/analsci.27.547.

Abstract

The extraction efficiency of a dispersive liquid-liquid microextraction (DLLME) method coupled with gas chromatography-microelectron capture detection (GC-µECD) for the simultaneous determination of 20 organochlorine pesticides (OCPs) in water samples was evaluated. The optimum conditions of DLLME for OCP measurement in water sample were determined with 10 µL of carbon tetrachloride (CCl(4)) and 1.5 mL of acetone as the extraction and dispersive solvents, respectively, all measurements were conducted under room temperature without the addition of salt. OCPs were extracted with good recoveries (60.35 - 107.89%) by the proposed method, except for heptachlor and aldrin due to the specific physico-chemical properties of these chemicals. Quantitative analysis showed that the relative standard deviations (RSDs) were below 9% and rather wider linear ranges (LRs) of 0.1 - 50 µg/L were obtained. The limits of detection (LODs) were in the range of 0.21 - 11.65 ng/L and no significant matrix effects were observed. Obtained results demonstrated that DLLME coupled with GC-µECD was rapid, convenient and efficient for OCP analysis in water samples.

摘要

评估了一种分散液液微萃取(DLLME)结合气相色谱 - 微电子捕获检测(GC - µECD)法同时测定水样中20种有机氯农药(OCPs)的萃取效率。确定了水样中OCP测量的DLLME最佳条件,分别以10 µL四氯化碳(CCl₄)和1.5 mL丙酮作为萃取和分散溶剂,所有测量均在室温下进行且不添加盐。所提出的方法对OCPs的萃取回收率良好(60.35 - 107.89%),但由于七氯和艾氏剂的特殊物理化学性质,这两种物质除外。定量分析表明,相对标准偏差(RSDs)低于9%,获得了0.1 - 50 µg/L较宽的线性范围(LRs)。检测限(LODs)在0.21 - 11.65 ng/L范围内,未观察到明显的基质效应。所得结果表明,DLLME结合GC - µECD用于水样中OCP分析快速、方便且高效。

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