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Separation of seventeen 2,3,7,8-substituted polychlorinated dibenzo-p-dioxins and dibenzofurans and 12 dioxin-like polychlorinated biphenyls by comprehensive two-dimensional gas chromatography with electron-capture detection
Umeå University, Faculty of Science and Technology, Department of Chemistry.
Umeå University, Faculty of Science and Technology, Department of Chemistry.
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2004 (English)In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1038, no 1-2, 189-199 p.Article in journal (Refereed) Published
Abstract [en]

Comprehensive two-dimensional gas chromatography (GC×GC) with electron-capture detection (ECD) has been optimized for the separation of seventeen 2,3,7,8-substituted polychlorinated dibenzo-p-dioxins and dibenzofurans and 12 dioxin-like polychlorinated biphenyls, with emphasis on the selection of the first- and second-dimension, commercially available, columns. When eight second-dimension columns were subsequently combined with a 100% methylpolysiloxane stationary phase (DB-1) in the first dimension to create orthogonal conditions, a complete separation of all congeners with different TEF values was obtained with two column combinations, DB-1 × VF-23 and DB-1 × LC-50. When other types of first-dimension columns were used (and orthogonality was partly sacrificed), a DB-XLB column combined with 007-65HT, VF-23 and LC-50 was found to provide a complete separation of all 29 priority congeners. Next, the potential of these three column combinations for real-life analysis was preliminarily studied. With a spiked and fractionated milk extract, DB-XLB × LC-50 was found to be the most powerful column combination, because of the good separation of the 29 priority congeners from each other as well as from the matrix constituents. Quantitative performance (close to three-order linearity; LODs, 30–150 fg injected; R.S.D.s, 1.5–6.5% (n=10)) was satisfactory.

Place, publisher, year, edition, pages
Amsterdam: Elsevier , 2004. Vol. 1038, no 1-2, 189-199 p.
Keyword [en]
Gas chromatography, comprehensive two-dimensional, Polychlorinated dibenzo-p-dioxins, Polychlorinated dibenzofurans, Dioxin-like polychlorinated biphenyls
Identifiers
URN: urn:nbn:se:umu:diva-14324DOI: 10.1016/j.chroma.2004.03.026OAI: oai:DiVA.org:umu-14324DiVA: diva2:153995
Available from: 2007-05-28 Created: 2007-05-28 Last updated: 2017-12-14Bibliographically approved
In thesis
1. Trace analysis of dioxins and dioxin-like PCBs using comprehensive two-dimensional gas chromatography with electron capture detection
Open this publication in new window or tab >>Trace analysis of dioxins and dioxin-like PCBs using comprehensive two-dimensional gas chromatography with electron capture detection
2006 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs), two groups of struc-turally related chlorinated aromatic hydrocarbons, generally referred to as “dioxins” are of great concern due to their extreme toxicity and presence in all compartments of the environment. Since they occur at very low levels, their analysis is complex and challenging, and there is a need for cost-efficient, reliable and rapid analytical alternatives to the expensive methods in-volving use of gas chromatography high-resolution mass spectrometry (GC-HRMS). It is im-portant to routinely monitor food and feed items to detect contaminations at an early stage. For the regulation of dioxins and dioxin-like PCBs in food and feed according to current legis-lation, large numbers of samples have to be analysed. Furthermore, soils at many industrial sites are also contaminated with dioxins and need remediation. In order to optimize the cost-efficiency of reclamation activities it is important to acquire information about the levels and distribution of dioxins in the contaminated areas.

The aim of the studies underlying this thesis was to investigate the potential of comprehen-sive two-dimensional gas chromatography with a micro-electron capture detector (GC × GC-µECD) as a cost-effective method for analysing dioxins and dioxin-like PCBs in food, feed, fly ash and contaminated soils. Quantification studies of dioxins and dioxin-like PCBs were con-ducted and results were compared with GC-HRMS reference data. Generally, there was good agreement between both the congener-specific results and data expressed as total toxic equiva-lents (TEQs). The developed GC × GC-µECD method meets the European Community (EC) requirements for screening methods for control of dioxins and dioxin-like PCBs in food and feed. The presented results also indicate that GC × GC-µECD has potential to be used as a routine method for the congener-specific analysis of 2,3,7,8-PCDD/Fs and dioxin-like PCBs in matrices such as food and feed, fly ash and soil.

However, to fully exploit the potential of the GC × GC-µECD technique, it should be combined with a fast and cost-efficient sample preparation procedure. Therefore, a number of certified reference materials (CRMs) were extracted using a new shape-selective pressurized liquid extraction technique with integrated carbon fractionation (PLE-C), and the purified extracts were analysed for PCDD/Fs using GC × GC-µECD. The results compared well with the certified values of a fly ash and a sandy soil CRM, but they were much too high for a com-plex clay soil CRM. It was concluded that this combination of techniques was very promising for screening ash and highly permeable soils.

Further assessments and method revisions are still required before GC × GC-µECD can be used on a routine basis, and available software packages need to be refined in order to accelerate the data-handling procedures, which currently restrict the sample throughput.

Place, publisher, year, edition, pages
Umeå: Kemi, 2006. 43 p.
Keyword
Comprehensive two-dimensional gas chromatography, GC × GC, µECD, PCDDs, PCDFs, dioxins, dioxin-like PCBs, Pressurized liquid extraction, PLE, PLE-C, food, feed, fly ash, soil
National Category
Environmental Sciences
Identifiers
urn:nbn:se:umu:diva-963 (URN)91-7264-234-3 (ISBN)
Public defence
2007-01-19, KB3B1, KBC, Umeå Universitet, Umeå, 10:00 (English)
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Supervisors
Available from: 2006-12-29 Created: 2006-12-29 Last updated: 2012-06-07Bibliographically approved

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