Solid-phase microextraction coupled with capillary electrophoresis for the determination of propranolol enantiomers in urine using a sol-gel derived calix[4]arene fiber

被引:63
作者
Zhou, XW
Li, XJ
Zeng, ZR [1 ]
机构
[1] Wuhan Univ, Dept Chem, Wuhan 430072, Peoples R China
[2] Hubei Normal Univ, Dept Chem & Environm Engn, Huangshi 435000, Peoples R China
基金
中国国家自然科学基金;
关键词
calix[4]arene; sol-gel; solid-phase microextraction; capillary electrophoresis; propranolol enantiomers; doping analysis;
D O I
10.1016/j.chroma.2005.11.126
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A new type of diglycidyloxy-calix[4]arene coated fiber made by sol-gel method was initially prepared for capillary electrophoresis (CE) sample pretreatment. By using headspace solid-phase microextraction (SPME) combined with a novel back-extraction facility coupled off-line to capillary zone electrophoresis (CZE), the simultaneous determination of propranolol enantiomers in human urine was achieved. The clean up effect and preconcentration effect were realized for the first time without derivatization during the SPME process in terms of these strong polarity and thermal stable compounds. Ultrasonic back-extraction and field amplified sample injection (FASI) technologies were employed. Extraction and back-extraction parameters were optimized. Preconcentration of the sample by calix[4]arene fiber based SPME and FASI increased the sensitivity, yielding a limit of detection (LOD) of 0.01 mu g/ml by CZE-diode array detection (DAD). Method repeatability (RSD < 6.5%) and fiber reusability (> 150 extraction procedures) were observedover a linear range (0.05-10 mu g/ml) in urine samples. Based on the superior thermal stability, high alkali- and solvent-resistant ability, marvelous repeatability and long lifetime of the novel fiber, this SPME-FASI-CZE procedure could meet the demand of minimum required performance limit (MRPL) set by the World Anti-doping Agency (WADA) for the detection of propranolol in urine samples. (c) 2005 Elsevier B.V. All rights reserved.
引用
收藏
页码:359 / 365
页数:7
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