色谱

色谱

• 样品预处理方法专栏 • 上一篇    下一篇

聚甲基三氟丙基硅氧烷固相微萃取涂层的制备及其对海水中酚类化合物的分析

观文娜,许峰,廉玫,徐媛,关亚风   

  1. Department of Instrumentation &Analytical Chemistry, Dalian Institute of

    Chemical Physics, the Chinese Academy of Sciences, Dalian 116023, China

  • 收稿日期:2007-08-14 修回日期:2007-08-21 出版日期:2007-09-30 发布日期:1985-03-25
  • 通讯作者: 关亚风

Poly(trifluoropropyl)methylsiloxane Coating for Solid-Phase

Microextraction and Its Application for the Analysis of Phenolic

Compounds in Sea Water

GUAN Wenna, XU Feng, LIAN Mei, XU Yuan, GUAN Yafeng   

  1. Department of Instrumentation &Analytical Chemistry, Dalian Institute of

    Chemical Physics, the Chinese Academy of Sciences, Dalian 116023, China

  • Received:2007-08-14 Revised:2007-08-21 Online:2007-09-30 Published:1985-03-25

PDF

968

摘要：

采用溶胶-凝胶技术制备了聚甲基三氟丙基硅氧烷(PTFPMS)涂层,并将其作为萃取

纤维针的萃取固定相。制备的涂层为多孔状结构,涂层厚度为10

μm。此涂层由于含有-C2H4CF3官能团,因此对电负性强的化合物具有高的选择性。最高

使用温度可达280 ℃,使用寿命可达150次。应用此涂层采用顶空固相微萃取方法分析了

海水样品中的酚类化合物。对影响萃取效率的萃取方式、萃取温度、萃取时间、离子强

度、pH值等萃取条件进行了优化。在优化条件下酚类化合物的检出限为0.02～1.2

μg/L。单根萃取纤维针的相对标准偏差(RSD,n=5)小于4.4%,用5根萃取纤维针萃取的RS

D小于15.7%,说明采用溶胶-凝胶技术制备的PTFPMS涂层有良好的重现性。

关键词: 酚类物质, 固相微萃取, 固相吸附搅拌棒, 海 水 , 聚甲基三氟丙基硅氧烷, 溶胶-凝胶

Abstract:

The poly(trifluoropropyl)methylsiloxane (PTFPMS) coating was

prepared as solid-phase microextraction (SPME) coating by sol-gel

technique. The coating has a porous microstructure and the thickness was

10 μm. Since the PTFPMS phase contains the functional group of -C2H4CF3,

it exhibits high affinity to compounds containing electron-attracting

groups. The PTFPMS phase can withstand desorption temperature up to 280

℃. The lifetime of the fiber SPME is more than 150 times. This coating

was used to analyse the phenolic compounds in water samples by head-space

solid-phase microextraction (HS-SPME) method. The parameters affecting

the extraction efficiency, such as extraction mode, extraction

temperature, extraction time, ion strength and pH, were optimized. The

limits of detection (LODs) of the method were 0.02-1.2 μg/L. The

relative standard deviations (RSDs) of single fiber and fiber-to-fiber

(n=5) were less than 4.4%, and 15.7%, respectively. The results indicated

that the sol-gel method has good repeatability for the preparation of the

PTFPMS coating.

Key words: phenolic compounds, poly(trifluoropropyl)methylsiloxane, sea water solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE), sol-gel technique