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CHROMATOGRAPHIC AND MASS SPECTRAL ANALYSES OF OLIGOSACCHARIDES AND INDIGO DYE EXTRACTED FROM COTTON TEXTILES WITH MANOVA AND ANOVA STATISTICAL DATA ANALYSES
Title
CHROMATOGRAPHIC AND MASS SPECTRAL ANALYSES OF OLIGOSACCHARIDES AND INDIGO DYE EXTRACTED FROM COTTON TEXTILES WITH MANOVA AND ANOVA STATISTICAL DATA ANALYSES.
Creator
Frisch, Jessica, Sigman, Michael, University of Central Florida
Abstract / Description
Research was conducted on thirteen 100% cotton denim samples using an acid wash, established by Murray, to extract oligosaccharides from the cellulosic material. The oligosaccharide ion groups (+, +, and +) for molecules with degrees of polymerization between two and seven (DP2-DP7) were analyzed using liquid chromatography coupled to mass spectrometry with an electrospray ionization interface (LC-ESI-MS). The results were compared using the least-squares means in a Multivariate ANOVA (MANOVA...
Show moreResearch was conducted on thirteen 100% cotton denim samples using an acid wash, established by Murray, to extract oligosaccharides from the cellulosic material. The oligosaccharide ion groups (+, +, and +) for molecules with degrees of polymerization between two and seven (DP2-DP7) were analyzed using liquid chromatography coupled to mass spectrometry with an electrospray ionization interface (LC-ESI-MS). The results were compared using the least-squares means in a Multivariate ANOVA (MANOVA) test followed by Univariate ANOVA and Tukey HSD tests and demonstrated that the method could correctly determine that two samples were statistically different 85.9% of the time when analyzing the amount (ng) of each of the oligosaccharide ion groups separately, and 82.0% when analyzing the total moles of monosaccharide units released. A dye extraction was performed on the denim materials and the extract analyzed using gas chromatography coupled with mass spectrometry (GC-MS). Indigo dye was present in all of the denim samples except one. When these results were combined with the two oligosaccharide statistical analyses, the discriminating power was increased to 88.5% and 85.9%, respectively. Additional cellulosic materials were also investigated including four white 100% cotton t-shirts as well as five raw cotton samples grown in Tajikistan, Uzbekistan, Egypt, Iran, and Benin West Africa. The analytical methodology gave results for the white cotton t-shirts and raw cotton samples that were inconsistent with those obtained from the denim samples.
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Date Issued
2008
Identifier
CFE0002068, ucf:47583
Format
Document (PDF)
PURL
http://purl.flvc.org/ucf/fd/CFE0002068
Tandem Mass Spectrometric Analysis of Ammonium and Sodium Oligoperoxide Adducts with the Application of Two-Dimensional Correlation Spectroscopy and Computational Chemistry
Title
Tandem Mass Spectrometric Analysis of Ammonium and Sodium Oligoperoxide Adducts with the Application of Two-Dimensional Correlation Spectroscopy and Computational Chemistry.
Creator
Frisch, Jessica, Sigman, Michael, Fookes, Barry, Hampton, Michael, University of Central Florida
Abstract / Description
Oligoperoxides, H[OO(CH3)2C]nOOH, are formed as side products in the synthesis of the primary high explosive triacetone triperoxide (TATP). Previous tandem mass spectrometry (MSn) experiments using a quadrupole ion trap reported that the open-chained oligoperoxide adducts of ammonium or sodium resulted in different product ions in the mass spectra. Dissociation mechanisms were previously proposed based on MSn experiments, where n(>)2; however, a dissociation pathway achieved by an MSn...
Show moreOligoperoxides, H[OO(CH3)2C]nOOH, are formed as side products in the synthesis of the primary high explosive triacetone triperoxide (TATP). Previous tandem mass spectrometry (MSn) experiments using a quadrupole ion trap reported that the open-chained oligoperoxide adducts of ammonium or sodium resulted in different product ions in the mass spectra. Dissociation mechanisms were previously proposed based on MSn experiments, where n(>)2; however, a dissociation pathway achieved by an MSn experiment, where n(>)2, may not necessarily be the same pathway achieved in an MS2 experiment. For this dissertation research, the collision induced dissociation pathways were investigated for the open-chained oligoperoxides in MS2 experiments utilizing a quadrupole ion trap. Tandem mass spectral experiments were performed for the open-chained oligoperoxides ranging from the trimer to the octamer (n=3-8), including both ammonium and sodium adducts. The dissociation pathways were proposed as a result of two-dimensional correlation spectroscopy applied to the mass spectral data, which was referred to as two-dimensional correlation mass spectrometry (2D-CMS). The 2D-CMS method was first validated by analysis of simple and more complex kinetic models followed by simple and more complex molecules. To further aid in the elucidation of the dissociation mechanisms, computational chemistry was performed for the optimization of stable precursor and product ion structures and calculations of their relative energies and adduct dissociation energies.
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Date Issued
2012
Identifier
CFE0004377, ucf:49371
Format
Document (PDF)
PURL
http://purl.flvc.org/ucf/fd/CFE0004377