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超声辅助离子液体分散液相微萃取-高效液相色谱法测定废水中雌激素的研究

Determination of Estrogens in Wastewater by Ultrasound-Assisted Ionic Liquid Dispersive Liquid-Phase Microextraction Coupled with High Performance Liquid Chromatography

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【作者】 刘美华邱彬陈国南陈曦

【Author】 LIU Mei-hua1,3,QIU Bin1,CHEN Guo-nan1,CHEN Xi1,2(1.Key Laboratory of Analysis and Detection Technology for Food Safety(Fuzhou University),Ministry of Education,Department of Chemistry,Fuzhou University,Fuzhou 350002,China;2.State Key Laboratory of Marine Environmental Science,Xiamen University,Xiamen 361005,China;3.Fuqing Branch of Fujian Normal University,Fuqing 350300,China)

【机构】 福州大学食品安全分析与检测教育部重点实验室化学化工学院福建师范大学福清分校厦门大学海洋环境科学国家重点实验室

【摘要】 将离子液体、分散液相微萃取与超声萃取技术结合,采用疏水性离子液体1-丁基-3-甲基咪唑六氟磷酸盐([C4 MIM][PF6])为萃取剂,建立了超声辅助离子液体分散液相微萃取-高效液相色谱法分析废水中3种雌激素物质(己烯雌酚、双烯雌酚、己烷雌酚)方法.试验采用50μL的离子液体,考察了溶液体积、溶液pH值、超声时间、静置时间、离心时间等因素对富集效果的影响.最佳的萃取条件为:溶液体积为6 mL,甲醇体积0.3 mL,溶液pH值为2.0,超声时间6min,静置时间30min,离心时间10 min.在优化的萃取条件下,3种雌激素的富集倍数可达到96.8~112.4倍;方法的线性范围为0.5-100.0μg/L;检出限为0.25~0.50μg/L.对浓度为5.0μg/L的3种物质测定6次的相对标准偏差为9.2%~10.8%.

【Abstract】 A novel method was established for the determination of estrogens in wastewater by ultrasonic assisted ionic liquid(1-butyl-3-methylimidazolium hexafluorophosphate,[C4MIM] \)dispersive liquid-phase microextraction coupled with high performance liquid chromatography.Some conditions that might affect the extraction efficiency,such as volume of solution,pH value of solution,ultrasonic time,hierarchical standing time,and centrifuging time were optimized.The results indicated that the optimal conditions were: 6 mL of solution at pH 2.0 for 6 min of ultrasonication,30 min of hierarchical standing and 10min of centrifugation.Under the above mentioned conditions,the extraction efficiency of ionic liquid based ultrasonic microextraction for the three estrogens were in the range of 96.8~112.4.Their linear ranges and detection limits were 0.5-100 μg/L and 0.25~0.50 μg/L respectively.The proposed method was applied to determine three estrogens in wastewater.The recoveries of three estrogens spiked in wastewater were in the range of 89.0%~96.6%.

  • 【文献出处】 分析测试技术与仪器 ,Analysis and Testing Technology and Instruments , 编辑部邮箱 ,2009年03期
  • 【分类号】X832
  • 【被引频次】32
  • 【下载频次】631
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