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Trace analysis of polychlorinated dibenzo-p-dioxins, dibenzofurans and WHO polychlorinated biphenyls in food using comprehensive two-dimensional gas chromatography with electron-capture detection
Umeå University, Faculty of Science and Technology, Chemistry.
Umeå University, Faculty of Science and Technology, Chemistry.
Umeå University, Faculty of Science and Technology, Chemistry.
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2005 (English)In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1086, no 1-2, 61-70 p.Article in journal (Refereed) Published
Abstract [en]

Trace analysis of 2,3,7,8-polychlorinated dibenzo-p-dioxins (PCDDs), dibenzofurans (PCDFs) and the 12 WHO-PCBs (four non-ortho and eight mono-ortho congeners that have been assigned toxic equivalence factors, TEFs, by the World Health Organisation) was conducted by comprehensive two-dimensional gas chromatography with a micro electron-capture detector (GC x GC-mu ECD). Four food matrices (fish oil from herring, spiked cows' milk, vegetable oil and an eel extract) were analysed by two GC x GC laboratories, and four GC-HRMS laboratories generated reference values. The two GC x GC laboratories used different column combinations for separating the target analytes. For the first dimension, non-polar DB-XLB and VF-1 columns were used, and for the second dimension, an LC-50 liquid crystalline column with unique selectivity for planar compounds. The congener-specific and total toxic equivalence (TEQ) data obtained using DB-XLB x LC-50 were in good agreement with results obtained by the GC-HRMS laboratories. The WHO-PCB data obtained with the VF-1 x LC-50 combination was also good, but the PCDD/F concentrations were sometimes overestimated due to matrix interferences. GC x GC-mu ECD using DB-XLB x LC-50 seems to fulfil the European Community requirements of a screening method for PCDD/F and WHO-PCB TEQ in food.

Place, publisher, year, edition, pages
2005. Vol. 1086, no 1-2, 61-70 p.
Keyword [en]
comprehensive two-dimensional gas chromatography, GC x GC, mu ECD; PCB, PCDD/F, TEF, TEQ, quantification, food, Dioxins, GC-HRMS
Identifiers
URN: urn:nbn:se:umu:diva-13351DOI: doi:10.1016/j.chroma.2004.11.071OAI: oai:DiVA.org:umu-13351DiVA: diva2:153022
Available from: 2007-05-08 Created: 2007-05-08 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)
Opponent
Supervisors
Available from: 2006-12-29 Created: 2006-12-29 Last updated: 2012-06-07Bibliographically approved

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