Comprehensive two-dimensional gas chromatography (GC x GC) measurements of volatile organic compounds in the atmosphere

Abstract. During the MINOS campaign in August 2001 comprehensive two-dimensional gas chromatography (GC×GC) was applied to the in situ measurements of atmospheric volatile organic compounds (VOCs) at the Finokalia ground station, Crete. The measurement system employs a thermal desorption unit for on-line sampling and injection, and a GC×GC separation system equipped with a flame ionization detector (FID) for detection. The system was optimized to resolve C7 − C14 organic components. Two-dimensional chromatograms from measurements of Finokalia air samples show several hundred wellseparated peaks. To facilitate peak identification, cartridge samples collected at Finokalia were analyzed using the same GC×GC system coupled with a time-of-flight mass spectrometer (TOF-MS). The resulting mass spectra were deconvoluted and compared to spectra from a database for tentative peak identification. About 650 peaks have been identified in the two-dimensional plane, with significant signal/noise ratios (>100) and high spectra similarities (>800). By comparing observed retention indices with those found in the literature, 235 of the identifications have been confirmed. 150 of the confirmed compounds show up in the C7 − C14 range of the chromatogram from the in situ measurement. However, at least as many peaks remain unidentified. For quantification of the GC×GC measurements, peak volumes of measured compounds have been integrated and externally calibrated using a standard gas mixture.

Comprehensive two-dimensional gas chromatography with atomic emission detection and correlation with mass spectrometric detection: principles and application in petrochemical analysis

Comprehensive gas chromatography (GC x GC) has been combined with atomic emission detection (AED) to enable element-selective detection. Under optimised experimental conditions, the requirement of minimum five data points across a peak can be obtained even for analytes eluting early from the second-dimension column. Simple manipulation of the results allows the combined presentation of up to four sets of elemental data in one two-dimensional plot. GC x GC with AED and mass spectrometric (MS) detection in petrochemical analysis for fingerprinting as well as the identification of N- and S-containing unknowns is presented as an application. © 2003 Elsevier B.V. All rights reserved

Identification of non-target compounds using gas chromatography with simultaneous atomic emission and mass spectrometric detection (GC-AED/MS): analysis of municipal wastewater.

Parallel atomic emission (AED) and mass spectrometric detection (MSD) was used for the gas chromatographic (GC) analysis of non-target compounds in influent and effluent water of a sewage treatment plant. Because of their potential environmental impact, non-target analysis was mainly focused on chlorinated compounds. With solid-phase extraction (SPE, styrene-divinylbenzene copolymer adsorbent) for analyte enrichment from 25 ml of aqueous sample, detection limits were 0.2-0.5 μg

Cytotoxicity of paracetamol and 3,5-dihalgenated analogues: Role of cytochrome P450 and formation of GSH conjugates and protein adducts.

The effect of 3,5-dihalogenation of paracetamol (PAR) on the cytotoxicity in rat hepatocytes isolated from 13-naphthoflavone pretreated, non-fasted rats, and the role of cytochrome P-450 in this regard, were studied. On incubation, 3,5-difluoro-PAR, 3,5-dichloro-PAR and 3,5-dibromo-PAR, as well as PAR, caused severe leakage of lactate dehydrogenase (LDH) which was preceded by a rapid concentration- and time-dependent depletion of intracellular glutathione (GSH). I

Attempt to unravel the composition of toxaphene by comprehensive two-dimensional gas chromatography with selective detection

Comprehensive two-dimensional gas chromatography (GCxGC) coupled with micro electron-capture and time-of-flight mass spectrometric (TOF-MS) detection has been used to analyse technical toxaphene. An HP-1xHT-8 column combination yielded highly structured chromatograms and revealed a complex mixture of over 1000 compounds what is significantly higher number than in any study before. The analysis of a mixture of 23 individual congeners and TOF-MS evaluation of technical toxaphene showed that the chromatogram is structured according to the number of chlorine substituents in a molecule. The nature of the compounds (bornane and camphene) does not appear to have any influence. The sum of the peak areas of all congeners in each group was calculated using laboratory-written software; based on these results, the composition of technical toxaphene as a function of the number of chlorine substituents was provisionally calculated and was found that hepta- and octachlorinated compounds represents 75 f the total toxaphene area

Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometric detection for the trace analysis of flavour compounds in food

The practicability and potential of comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC-TOF-MS) for the analysis of complex flavour mixtures in food were studied. With the determination of key flavour targets in dairy samples as an example, it was demonstrated that GC×GC dramatically improves the separation. As a consequence, identification and, more importantly, quantification down to the ng/g level can be performed more reliably: background interferences largely disappear. Next to the peak table generated from the GC-TOF-MS software after data processing, the additional use of well-ordered patterns in the 2D-plane and information from second-dimension retention times can substantially help the identification of unknowns. The technique was successfully used for an evaluation of extraction techniques and the characterisation of different types of samples. © 2003 Published by Elsevier B.V