应用化学

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自制离子液体固相微萃取涂层分析人体尿液中的五氯酚

胡庆兰   

  1. (湖北第二师范学院化学与生命科学学院 武汉 430205)
  • 收稿日期:2012-04-24 修回日期:2012-05-25 出版日期:2013-03-10 发布日期:2013-03-10
  • 通讯作者: 胡庆兰,高级工程师; Tel:027-87943697; Fax:027-87680863; E-mail:huqinglan_123@163.com; 研究方向:色谱分析
  • 基金资助:
    湖北第二师范学院重点学科建设应用化学项目资助

Determination of Pentachlorophenol in Human Urine by Homemade Ionic liquid Solid-phase Microextraction Coating

HU Qinglan   

  1. (School of Chemistry and Life Sciences,Hubei University of Education,Wuhan 430205,China)
  • Received:2012-04-24 Revised:2012-05-25 Published:2013-03-10 Online:2013-03-10
  • Contact: hu

摘要: 建立了顶空固相微萃取与气相色谱法(HS-SPME-GC)测定人体尿液中五氯酚(PCP)的新方法。 采用溶胶-凝胶法,加入自制的离子液体键合固相微萃取涂层,优化了萃取温度、萃取时间、pH值、离子强度及解吸时间。 结果表明,样品中加入3 g NaCl,溶液的pH值为2,并以一定速度搅拌的条件下,在80 ℃顶空萃取50 min,300 ℃下解吸5 min,方法的检测限为5.0 ng/L,线性范围为0.05~100 μg/L,相对标准偏差(RSD)为5.9%,加标回收率为106.6%。

关键词: 固相微萃取, 气相色谱, 溶胶-凝胶法, 五氯酚, 尿液

Abstract: A new method for the determination of pentachlorophenol(PCP) in human urine has been developed by headspace solid-phase microextraction with gas chromatography(HS-SPME-GC). A homemade ionic liquid(IL) bonded coating solid-phase microextraction was added by the sol-gel method. The extraction conditions were optimized as the extraction temperature of 80 ℃, extraction time of 50 min by headspace, desorption time of 5 min at 300 ℃, NaCl amount of 3 g, pH of 2 and under stirring. The detection limits was 5.0 ng/L. The linear range was 0.05~100 μg/L. The relative standard deviations(RSD) was 5.9%. The recovery was 106.6%.

Key words: solid- phase microextraction, gas chromatography, sol-gel method, pentachlorophenol, urine

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