光谱学与光谱分析 |
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On-Line Coupling of Microcolumn Electrophoresis and UV-Vis Spectrophotometry |
LI Lian, HE You-zhao*, GAN Wu-er, WANG Xiao-kui, XIE Hai-yang, GAO Yong |
Department of Chemistry, University of Science and Technology of China, Hefei 230026, China |
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Abstract In the present paper, a laboratory-made high-performance electrophoresis microcolumn unit was prepared for UV-Vis spectrophotometer. X-ray diffraction was used in the preparation of electrophoretic microcolumns. And an analytical technique of microcolumn electrophoresis coupled with UV-Vis spectrophotometry was introduced. Uniform quartz microncrystals were prepared by hydrothermal synthesis. Their crystalline phase and morphology were identified by X-ray diffraction and scanning electron microscope, respectively. The quartz microncrystals were packed into a 2-mm i.d. fused-silica tube to prepare the electrophoretic microcolumn. With 1.5 mmol·L-1 disodium phosphate buffer solution (pH 11.5) containing 25% (φ) methanol and 10% (φ) acetonitrile, tryptophan, phenylalanine and tyrosine were on-line separated on line and detected by microcolumn electrophoresis coupled with UV-Vis spectrophotometry without derivatization. The limits of detection were 0.037, 0.20 and 0.20 μmol·L-1, respectively. The separation efficiency of tryptophan was 4.5×104 plates/m. The sample capacity of the electrophoretic microcolumn achieved 35 μL. It was found that the electrophoretic microcolumn packed with quartz microncrystals was able to limit Joule heat, increase sample capacity and enhance detection sensitivity. The laboratory-made electrophoretic microcolumn could be a high-performance separation unit for conventional UV-Vis spectrophotometer. The on-line coupling of microcolumn electrophoresis and UV-Vis spectrophotometry could separate and determine samples with complicated matrices, reduce zone broadening and enhance separation efficiency, so expand the analytical function of spectrophotometer in the trace analysis of mixed components with overlapped spectra.
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Received: 2009-02-26
Accepted: 2009-05-28
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Corresponding Authors:
HE You-zhao
E-mail: yzhe@ustc.edu.cn
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