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1.
Anal Chem ; 68(19): 3441-9, 1996 Oct 01.
Artigo em Inglês | MEDLINE | ID: mdl-8843141

RESUMO

Continuous zone electrophoretic separations in narrow channels coupled to small-bore capillaries have been demonstrated and characterized previously. Presented here is the use of this new technique to monitor dynamic chemical changes occurring in a flow injection analysis system. The fundamental aspects of the data that this type of separation generates are discussed in a comparison of static and dynamic analyses. An analysis of a dynamic separation is also provided to thoroughly outline the steps necessary to deconvolute the data. Three types of dynamic analyses, which simulate realistic analytical situations, are then examined in detail. The first of these involves the addition of a mixture of four dansylated amino acids to the flow injection system to provide several different sample duration periods. The second is the staggered addition of short-duration plugs of analyte to the system. The third is the continuous addition of one analyte at different concentrations. Quantitative information generated by these experiments includes the simultaneous determination of the time of analyte contact and its duration of contact with the sampling capillary, identification of analytes based on electrophoretic mobilities, and concentration changes with time. For the addition of a 1.52 mM solution of N epsilon-dansyl-L-lysine, the sample duration and time of analyte contact with the capillary was determined with an error of < 4%. Concentration changes in the FIA system of dansyl-L-arginine over the range of 0.38-3.04 mM are also demonstrated with transitional edges on the time scale of 3-4 s. Qualitatively, the appearance of analyte bands can reveal impurities and fronting or tailing effects as seen in conventional capillary electrophoretic separations. The results demonstrate the ability of the technique to successfully probe dynamic environments.


Assuntos
Eletroforese Capilar/métodos , Arginina/análogos & derivados , Arginina/química
3.
Anal Chem ; 65(22): 3313-9, 1993 Nov 15.
Artigo em Inglês | MEDLINE | ID: mdl-8291681

RESUMO

Continuous zone electrophoretic separations in channels have been demonstrated. This new technique has the potential to continuously sample and separate analytes from volume-limited microenvironments. A small-bore capillary is used to electrophoretically sample, but not separate, a mixture of dansylated amino acids. The capillary is coupled to a quartz channel structure in a manner which allows continuous injection of the sampled material into the channel. The channel functions to continuously separate the sampled material via electrophoresis. A laser-induced fluorescence detection scheme, which involves two fiber optic arrays situated at the channel exit, monitors eluting analytes. A continuous separation of dansylated amino acids on the time scale of a few minutes demonstrates the utility of the technique. Sampling has been performed continuously up to 400 s, and initial detection limits are approximately 30 microM.


Assuntos
Compostos de Dansil/isolamento & purificação , Eletroforese/métodos , Lisina/análogos & derivados , Lasers , Lisina/isolamento & purificação , Espectrometria de Fluorescência
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