Please use this identifier to cite or link to this item:
http://hdl.handle.net/11375/19331
Title: | The Combination of Microbore Liquid Chromatography and Mass Spectrometry |
Authors: | Gergely, Robert John |
Advisor: | Quilliam, M. A. |
Department: | Chemistry |
Keywords: | combination, mictobore, liquid, chromatography, mass, spectrometry, calibration |
Publication Date: | Mar-1986 |
Abstract: | <p> An inexpensive method was developed for the conversion of a high performance liquid chromatography (HPLC) system for use with 1 mm I.D. microbore columns. Chromatographic performance of the system was tested under both isocratic and gradient elution conditions, using a standard mixture of 16 polycyclic aromatic hydrocarbons (PAH).</p> <p> The microbore column HPLC was also coupled to a mass spectrometer equipped with a moving belt interface. Chromatographic performance under isocratic and gradient elution and mass spectral performance under scanning and selected ion monitoring modes were tested using the PAH standard.</p> <p> A marine sediment extract was subjected to qualitative and quantitative analysis for PAH. Qualitative results on the sample were obtained from a combination of retention indices, mass spectra, and retention times. Quantitation was performed by microbore column liquid chromatography-mass spectrometry (LC/MS) in the selected ion monitoring mode of operation. The method of calibration used was external calibration.</p> <p> The microbore column HPLC system exhibited good chromatographic behavior. Resolution, peak shape and short term retention time reproducibility were good, although, long term retention time fluctuations, due to changing mobile phase flow rates, were noted.</p> <p> The combination of microbore column HPLC with a moving belt interface and mass spectrometer gave excellent results. Problems commonly encountered with conventional column (4.6 mm I.D.) LC/MS, such as backstreaming, droplet formation, and splattering were greatly reduced, resulting in no apparent loss of chromatographic integrity and stable mass spectrometer operating conditions. These operating conditions proved to be most advantageous in the quantitative analysis of the marine sediment extract by selected ion monitoring.</p> |
URI: | http://hdl.handle.net/11375/19331 |
Appears in Collections: | Open Access Dissertations and Theses |
Files in This Item:
File | Description | Size | Format | |
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Gergely_Robert_J._1986Mar_Masters..pdf | 2.56 MB | Adobe PDF | View/Open |
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