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Title: Capillary liquid chromatography using laser-based and mass spectrometric detection. Final technical progress report, September 1, 1989--January 31, 1993

Abstract

In the years following the 1986 seminal paper (J. Chromatogr. Sci., 24, 347-352) describing modern capillary zone electrophoresis (CZE), the prominence of capillary electrokinetic separation techniques has grown. A related electrochromatographic technique is micellar electrokinetic capillary chromatography (MECC). This report presents a brief synopsis of research efforts during the current 3-year period. In addition to a description of analytical separations-based research, results of efforts to develop and expand spectrometric detection for the techniques is reviewed. Laser fluorometric detection schemes have been successfully advanced. Mass spectrometric research was less fruitful, largely owing to personnel limitations. A regenerable fiber optic sensor was developed that can be used to remotely monitor chemical carcinogens, etc. (DLC)

Authors:
;
Publication Date:
Research Org.:
Tennessee Univ., Knoxville, TN (United States). Dept. of Chemistry
Sponsoring Org.:
USDOE, Washington, DC (United States)
OSTI Identifier:
10182289
Report Number(s):
DOE/ER/13613-36
ON: DE92040524
DOE Contract Number:
FG05-86ER13613
Resource Type:
Technical Report
Resource Relation:
Other Information: PBD: [1992]
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; 59 BASIC BIOLOGICAL SCIENCES; ELECTROPHORESIS; OPTIMIZATION; FULLERENES; LIQUID COLUMN CHROMATOGRAPHY; POLYCYCLIC AROMATIC HYDROCARBONS; PROGRESS REPORT; CAPILLARY FLOW; LASER SPECTROSCOPY; MICELLAR SYSTEMS; IMMUNOASSAY; OPTICAL FIBERS; ANTIBODIES; FLUORESCENCE SPECTROSCOPY; DERIVATIZATION; CHEMILUMINESCENCE; 400105; 550200; SEPARATION PROCEDURES; BIOCHEMISTRY

Citation Formats

Sepaniak, M.J., and Cook, K.D. Capillary liquid chromatography using laser-based and mass spectrometric detection. Final technical progress report, September 1, 1989--January 31, 1993. United States: N. p., 1992. Web. doi:10.2172/10182289.
Sepaniak, M.J., & Cook, K.D. Capillary liquid chromatography using laser-based and mass spectrometric detection. Final technical progress report, September 1, 1989--January 31, 1993. United States. doi:10.2172/10182289.
Sepaniak, M.J., and Cook, K.D. 1992. "Capillary liquid chromatography using laser-based and mass spectrometric detection. Final technical progress report, September 1, 1989--January 31, 1993". United States. doi:10.2172/10182289. https://www.osti.gov/servlets/purl/10182289.
@article{osti_10182289,
title = {Capillary liquid chromatography using laser-based and mass spectrometric detection. Final technical progress report, September 1, 1989--January 31, 1993},
author = {Sepaniak, M.J. and Cook, K.D.},
abstractNote = {In the years following the 1986 seminal paper (J. Chromatogr. Sci., 24, 347-352) describing modern capillary zone electrophoresis (CZE), the prominence of capillary electrokinetic separation techniques has grown. A related electrochromatographic technique is micellar electrokinetic capillary chromatography (MECC). This report presents a brief synopsis of research efforts during the current 3-year period. In addition to a description of analytical separations-based research, results of efforts to develop and expand spectrometric detection for the techniques is reviewed. Laser fluorometric detection schemes have been successfully advanced. Mass spectrometric research was less fruitful, largely owing to personnel limitations. A regenerable fiber optic sensor was developed that can be used to remotely monitor chemical carcinogens, etc. (DLC)},
doi = {10.2172/10182289},
journal = {},
number = ,
volume = ,
place = {United States},
year = 1992,
month = 9
}

Technical Report:

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  • CLG was studied for the analysis of small, complex samples and of difficult-to-resolve compounds. Optical and mass spectrometric detection for CLG was also studied. Emphasis was on micellar electrokinetic capillary chromatography. Biological materials have been successfully separated. (DLC)
  • The focus of this work is the development of capillary liquid chromatography, in particular an electrokinetic separation technique that we have termed micellar electrokinetic capillary chromatography (MECC), as a practical separation technique for the analyses of volume-limited complex samples and for difficult-to-resolve compounds. Most of our research during this period has involved fundamental and practical studies of the MECC technique. Solutes are separated in MECC in open capillary columns based upon their differential distribution between an electroosmotically-pumped mobile phase and an electrophoretically-retarded micellar phase. In our work the electrophoretic flow of the micelles opposes and is of a smaller magnitudemore » than the electroosmotic flow. Consequently, solutes that partition between the mobile and micellar phases are eluted within a limited retention range. The main virtues of the MECC technique are exceptional efficiency and the fact that it can be used to separate samples containing charged, neutral, or mixtures of charged and neutral solutes. The restriction of solutes demonstrating at least moderate water solubility and the limited elution range of the technique are limitations of MECC. 13 refs.« less
  • In the years following the 1986 seminal paper (J. Chromatogr. Sci., 24, 347-352) describing modern capillary zone electrophoresis (CZE), the prominence of capillary electrokinetic separation techniques has grown. A related electrochromatographic technique is micellar electrokinetic capillary chromatography (MECC). This report presents a brief synopsis of research efforts during the current 3-year period. In addition to a description of analytical separations-based research, results of efforts to develop and expand spectrometric detection for the techniques is reviewed. Laser fluorometric detection schemes have been successfully advanced. Mass spectrometric research was less fruitful, largely owing to personnel limitations. A regenerable fiber optic sensor wasmore » developed that can be used to remotely monitor chemical carcinogens, etc. (DLC)« less
  • The research performed during the past year has mainly focused on investigating and minimizing the problems listed below that limit the practical utility of these capillary electrokinetic separation techniques in chemical analysis. (1) Analyses are hindered by poor reproducibility. This is largely a result of complicated and irreproducible capillary wall-solute interactions that often result in adsorption and mobility changes. (2) While the Micellar Electrokinetic Capillary Chromatography technique permits the separations of neutral solutes, hydrophobic compounds are difficult to separate and manipulation of capacity factors is critically important due to a limited elution range. Because of the limited elution range, itmore » is also beneficial to enhance separation selectivity through the use of non-traditional surfactants. (3) The very small solute band volumes require that on-column'' detection be performed (usually optical detection) and this seriously limits detectability. Laser fluorimetry is particularly amenable to on- column detection with these capillary separation technique. We have explored methods of on-column labeling and multi-wavelength detection to expand the utility of this mode of detection. 35 refs., 7 figs.« less
  • The DOE-supported research performed during the past year has mainly focused on investigating and minimizing three problems that limit the practical utility of these capillary electrokinetic separation techniques in chemical analysis. (1) Analyses are hindered by poor reproducibility. This is largely a result of complicated and irreproducible capillary wall-solute interactions that often result in adsorption and mobility changes. (2) While the (micellar electrokinetic capillary chromatography) (MECC) technique permits the separations of neutral solutes, hydrophobic compounds are difficult to separate and manipulation of capacity factors (k's) is critically important. (3) The very small solute band volumes require that on-column detection bemore » performed (usually optical detection) and this seriously limits detectability. In addition to these projects, the electrokinetic equivalent of affinity chromatography and development of remote fiber-optic sensors to measure chemical carcinogens and other compounds have been investigated. 5 refs., 2 figs.« less