This study examines how the height and width of peaks exiting the secondary column of a comprehensive two-dimensional gas chromatography (GC × GC) separation are affected by the width of the pulse introduced to the secondary column. A flow-modulated GC × GC apparatus was assembled that allowed input pulse widths to be controlled precisely over a range of 10 to 70 ms. GC × GC chromatograms were obtained using secondary columns containing a polyethylene glycol stationary phase with internal diameters of 0.
View Article and Find Full Text PDFA fluidic device called the multi-mode modulator (MMM) has been developed for use as a comprehensive two-dimensional gas chromatography (GC x GC) modulator. The MMM can be employed in a wide range of capacities including as a traditional heart-cutting device, a low duty cycle GC x GC modulator, and a full transfer GC x GC modulator. The MMM is capable of producing narrow component pulses (widths <50ms) while operating at flows compatible with high resolution chromatography.
View Article and Find Full Text PDFJ Chromatogr A
November 2015
Comprehensive two-dimensional gas chromatography (GC×GC) modulators normally transfer primary column effluent to the head of the secondary column as a series of sharp pulses. Such pulses are produced with time-varying temperature gradients in thermal modulation or with time-varying flow patterns in flow modulation. Thermal modulators produce narrow peaks at optimal flow rates, but require large amounts of consumables or a highly engineered heating/cooling system.
View Article and Find Full Text PDFA comprehensive two-dimensional gas chromatography (GC×GC) method for separating siloxanes from hydrocarbons has been developed using a systematic process. First, the retention indices of a set of siloxanes and a set of hydrocarbons were determined on 6 different stationary phases. The retention indices were then used to model GC×GC separation on 15 different stationary phase pairs.
View Article and Find Full Text PDFThe iterative trapping method has been developed for concentrating gaseous volatile organic compounds (VOCs) prior to gas chromatographic analysis. VOCs are trapped in a 50 cm × 0.53 mm metal capillary column coated with a 7 μm thick film of polydimethylsiloxane (PDMS).
View Article and Find Full Text PDFA new high-speed valve-based modulator has been designed and tested for use in comprehensive two-dimensional gas chromatography (GC×GC). The modulator is a Deans switch constructed from two micro-volume fittings and a solenoid valve. Modulator performance was characterized over a wide range of device settings including the magnitude of the switching flow, the gap between the tips of the primary and secondary column, the primary column flow rate, and the carrier gas identity.
View Article and Find Full Text PDFThe GC×GC solvation parameter model has been used to identify effective stationary phases for the separation of fatty acid methyl esters (FAMEs) from petroleum hydrocarbons. This simple mathematical model was used to screen the 1225 different combinations of 50 stationary phases. The most promising pairs combined a poly(methyltrifluoropropylsiloxane) stationary phase with a poly(dimethyldiphenylsiloxane) stationary phase.
View Article and Find Full Text PDFA comprehensive 2-D GC (GC x GC) instrument equipped with a flow-switching modulator was used to determine the concentration of ethanol and eight other alcohols in a retail pump sample of E85 fuel. E85 is a mixture of ethanol and gasoline where the ethanol concentration can range from 70 to 85 vol%. The increased peak capacity and selectivity generated by GC x GC analysis allowed the alcohols to be fully resolved from the gasoline hydrocarbons.
View Article and Find Full Text PDFA solvation parameter model was used to generate comprehensive two-dimensional gas chromatography (GC x GC) retention diagrams for 54 solutes on four different stationary phase combinations. Retention diagrams are plots used to predict the relative position of solutes in GC x GC chromatograms. In this study, retention diagrams were based entirely on solute and stationary phase descriptors taken from the literature.
View Article and Find Full Text PDFA flow-switching two-dimensional gas chromatography (GCxGC) apparatus has been constructed that can operate at temperatures as high as 340 degrees C. This system is employed to analyze complex hydrocarbon mixtures such as diesel fuel, gas-oil, motor oil, and petroleum contaminated environmental samples. The GCxGC system generates two-dimensional chromatograms with minimal overlap between the aliphatic and aromatic regions This allows these compound classes to be independently quantitated without prior fractionation.
View Article and Find Full Text PDFComprehensive two-dimensional gas chromatography (GCxGC) is used to analyze petroleum diesel, biodiesel, and biodiesel/petroleum diesel blends. The GCxGC instrument is assembled from a conventional gas chromatograph fitted with a simple, in-line fluidic modulator. A 5% phenyl polydimethylsiloxane primary column is coupled to a polyethylene glycol secondary column.
View Article and Find Full Text PDFA high-temperature ionic liquid, trihexyl(tetradecyl)phosphonium bis(trifluoromethane)sulfonamide, was used as the primary column stationary phase for comprehensive two-dimensional gas chromatography (GC x GC). The ionic liquid (IL) column was coupled to a 5% diphenyl/95% dimethyl polysiloxane (HP-5) secondary column. The retention characteristics of the IL column were compared to polyethylene glycol (DB-Wax) and 50% phenyl/50% methyl polysiloxane (HP-50+).
View Article and Find Full Text PDFJ Chromatogr A
November 2007
A model for approximating the relative retention of solutes in comprehensive two-dimensional gas chromatography (GCxGC) is presented. The model uses retention data from standard single-column temperature-programmed separations. The one-dimensional retention times are first converted into retention indices and then these indices are combined in a simple manner to generate a retention diagram.
View Article and Find Full Text PDFA microfluidic Deans switch was used as a comprehensive two-dimensional gas chromatography (GCxGC) modulator. The simplicity and wide temperature range of the Deans switch make it a promising alternative to existing modulation techniques. However, the Deans switch is a low duty cycle modulator; that is, it samples only a small portion of the primary column effluent.
View Article and Find Full Text PDFThe oxidation of linoleic acid produces several products with biological activity including the hydroperoxy fatty acid 13-hydroperoxyoctadecadienoic acid (13-HPODE), the hydroxy fatty acid 13-hydroxyoctadecadienoic acid (13-HODE), and the 2,4-dienone 13-oxooctadecadienoic acid (13-OXO). In the present work, the peroxidase activity of glutathione transferases (GST) A1-1, M1-1, M2-2, and P1-1(Val 105) toward 13-HPODE has been examined. The alpha class enzyme is the most efficient peroxidase while the two enzymes from the mu class exhibit weak peroxidase activity toward 13-HPODE.
View Article and Find Full Text PDFComprehensive two-dimensional chromatography generates a two-dimensional chromatogram from a one-dimensional signal array. This process can only be done unambiguously when the range of secondary retention times is less than the modulation period. However, complex samples often produce wider ranges of secondary retention times.
View Article and Find Full Text PDFClin Orthop Relat Res
March 2004
Polymethylmethacrylate bone cement beads impregnated with antibiotic are a common treatment for patients with persistent articular joint infections or osteomyelitis. They also are used as a prophylaxis for infection in patients with large soft tissue wounds. The current study was designed to evaluate the relationship between bead geometry and elution of the antibiotic tobramycin by methodically varying the shape of the beads for a given set of volumes.
View Article and Find Full Text PDFThe oxidation of linoleic acid leads to the generation of several products with biological activity, including 13-oxooctadeca-9,11-dienoic acid (13-OXO), a bioactive 2,4-dienone that has been linked to cell differentiation. In the current work, the conjugation of 13-OXO by human glutathione transferases (GSTs) of the alpha (A1-1, A4-4), mu (M1-1, M2-2) and pi (the allelic variants P1-1/ile, and P1-1/val) classes, and a rat theta (rT2-2) class enzyme has been evaluated. The kinetics and stereoselectivity of the production of the 13-OXO-glutathione conjugate (13-OXO-SG) have been examined.
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