Comparative Study Of The Utility Of Electron Ionization And Chemical Ionization Mass Spectrometry For Confirmation And Quantification Of Stimulants In Urine

An analytical procedure for the detection of stimulants in urine using gas chromatography-mass spectrometry (GC-MS) is one of the analytical challenges facing anti-doping laboratories. The use of derivatising reagents for the target compounds will provide better peak shapes, reduce the polarity and...

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Main Author:	Almeer, Muna Ahmad M A
Format:	Thesis
Language:	English
Published:	2013
Subjects:	RS1-441 Pharmacy and materia medica
Online Access:	http://eprints.usm.my/46171/1/Muna%20Ahmad%20M%20A%20Almeer24.pdf
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id	my-usm-ep.46171
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spelling	my-usm-ep.461712020-02-11T04:07:49Z Comparative Study Of The Utility Of Electron Ionization And Chemical Ionization Mass Spectrometry For Confirmation And Quantification Of Stimulants In Urine 2013-11 Almeer, Muna Ahmad M A RS1-441 Pharmacy and materia medica An analytical procedure for the detection of stimulants in urine using gas chromatography-mass spectrometry (GC-MS) is one of the analytical challenges facing anti-doping laboratories. The use of derivatising reagents for the target compounds will provide better peak shapes, reduce the polarity and enhance the gas chromatographic properties, providing a good separation and mass spectra with high abundance for both identification and quantitative analysis, thus enhancing the detectability of a compound. Silylation, acylation and alkylation reactions are the most effective and common derivatization methods that are used for the GC. This research was focused on five banned stimulants from the WADA prohibited list which were amphetamine, methamphetamine, ephedrine, methylephedrine and cathine. When these compounds were derivatised with various derivatising reagents the limits of detection can be lowered considerably. Traditional GC/MS using electron impact ionisation suffers from product of low mass fragment ions making confirmation of these analytes difficult. When these derivatised compounds were analysed using chemical ionisation (CI) in the GC-MS, the protonated ion [M+H]+ as well as the [M+29]+ and [M+41]+ ions were obtained to be used as confirmatory ions. This research showed that using two steps derivatization by MSTFA followed by MBTFA and analysis using chemical ionisation (CI) can fulfil the identification criteria for qualitative identification of compounds in line with the WADA criteria. 2013-11 Thesis http://eprints.usm.my/46171/ http://eprints.usm.my/46171/1/Muna%20Ahmad%20M%20A%20Almeer24.pdf application/pdf en public masters Universiti Sains Malaysia Pusat Pengajian Sains Farmasi
institution	Universiti Sains Malaysia
collection	USM Institutional Repository
language	English
topic	RS1-441 Pharmacy and materia medica
spellingShingle	RS1-441 Pharmacy and materia medica Almeer, Muna Ahmad M A Comparative Study Of The Utility Of Electron Ionization And Chemical Ionization Mass Spectrometry For Confirmation And Quantification Of Stimulants In Urine
description	An analytical procedure for the detection of stimulants in urine using gas chromatography-mass spectrometry (GC-MS) is one of the analytical challenges facing anti-doping laboratories. The use of derivatising reagents for the target compounds will provide better peak shapes, reduce the polarity and enhance the gas chromatographic properties, providing a good separation and mass spectra with high abundance for both identification and quantitative analysis, thus enhancing the detectability of a compound. Silylation, acylation and alkylation reactions are the most effective and common derivatization methods that are used for the GC. This research was focused on five banned stimulants from the WADA prohibited list which were amphetamine, methamphetamine, ephedrine, methylephedrine and cathine. When these compounds were derivatised with various derivatising reagents the limits of detection can be lowered considerably. Traditional GC/MS using electron impact ionisation suffers from product of low mass fragment ions making confirmation of these analytes difficult. When these derivatised compounds were analysed using chemical ionisation (CI) in the GC-MS, the protonated ion [M+H]+ as well as the [M+29]+ and [M+41]+ ions were obtained to be used as confirmatory ions. This research showed that using two steps derivatization by MSTFA followed by MBTFA and analysis using chemical ionisation (CI) can fulfil the identification criteria for qualitative identification of compounds in line with the WADA criteria.
format	Thesis
qualification_level	Master's degree
author	Almeer, Muna Ahmad M A
author_facet	Almeer, Muna Ahmad M A
author_sort	Almeer, Muna Ahmad M A
title	Comparative Study Of The Utility Of Electron Ionization And Chemical Ionization Mass Spectrometry For Confirmation And Quantification Of Stimulants In Urine
title_short	Comparative Study Of The Utility Of Electron Ionization And Chemical Ionization Mass Spectrometry For Confirmation And Quantification Of Stimulants In Urine
title_full	Comparative Study Of The Utility Of Electron Ionization And Chemical Ionization Mass Spectrometry For Confirmation And Quantification Of Stimulants In Urine
title_fullStr	Comparative Study Of The Utility Of Electron Ionization And Chemical Ionization Mass Spectrometry For Confirmation And Quantification Of Stimulants In Urine
title_full_unstemmed	Comparative Study Of The Utility Of Electron Ionization And Chemical Ionization Mass Spectrometry For Confirmation And Quantification Of Stimulants In Urine
title_sort	comparative study of the utility of electron ionization and chemical ionization mass spectrometry for confirmation and quantification of stimulants in urine
granting_institution	Universiti Sains Malaysia
granting_department	Pusat Pengajian Sains Farmasi
publishDate	2013
url	http://eprints.usm.my/46171/1/Muna%20Ahmad%20M%20A%20Almeer24.pdf
_version_	1747821625751896064

Comparative Study Of The Utility Of Electron Ionization And Chemical Ionization Mass Spectrometry For Confirmation And Quantification Of Stimulants In Urine

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