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Comparative assessment of the chromatographic separation of 2,3,7,8-substituted polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans using supercritical fluid chromatography and high resolution gas chromatography
Örebro University, School of Science and Technology. Wellington Laboratories Inc., Guelph, Canada.
Örebro University, School of Science and Technology.ORCID iD: 0000-0001-6217-8857
Örebro University, School of Science and Technology.ORCID iD: 0000-0002-6330-789X
Chemistry Department, University of Guelph, Guelph, ON, Canada.
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2015 (English)In: Analytical Methods, ISSN 1759-9660, E-ISSN 1759-9679, Vol. 7, no 21, 9245-9253 p.Article in journal (Refereed) Published
Abstract [en]

The analysis of legacy environmental contaminants, such as polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs), using high resolution gas chromatography (HRGC) is well established and universally accepted. The use of an alternative separation technique, such as packed column supercritical fluid chromatography (pSFC), may be of interest as a fast, green, and cost effective method of analyzing environmental samples. The technique is amenable to a broad range of chemical compounds and could facilitate the simultaneous analysis of multiple compound classes as well as the inclusion of thermally labile compounds in a single targeted analysis. The recent re-emergence of this technology due to the introduction of more robust and efficient instrumentation may result in an increased acceptance of pSFC analytical techniques in this area. Herein, the first reported analytical separation of PCDDs and PCDFs by pSFC is described and its separation capabilities are compared with established HRGC protocols. Elution profiles of 2,3,7,8-substituted PCDDs and PCDFs were examined and the separation of PCDD/PCDF homologue groups was found to be comparable to those accomplished using HRGC. Similarly, the resolution of tetrachlorodibenzo-p-dioxin (TCDD) congeners, as required by current regulatory methods utilizing HRGC, was demonstrated and the separation of possible co-eluting PCDD/PCDF congeners was examined and compared to that achieved using popular HRGC capillary columns. The possibility of concurrent analysis of toxic polychlorinated biphenyls (PCBs) with PCDDs and PCDFs using the developed pSFC method was also investigated. The effective separation of these environmental contaminants obtained using pSFC and subsequent detection utilizing atmospheric pressure photoionization tandem mass spectrometry at environmentally relevant levels demonstrates the promise associated with this technique for the analysis of environmental extracts.

Place, publisher, year, edition, pages
Royal Society of Chemistry, 2015. Vol. 7, no 21, 9245-9253 p.
National Category
Chemical Sciences Food Science
Research subject
Chemistry
Identifiers
URN: urn:nbn:se:oru:diva-46699DOI: 10.1039/c5ay01644dISI: 000363732900034Scopus ID: 2-s2.0-84945421701OAI: oai:DiVA.org:oru-46699DiVA: diva2:873198
Available from: 2015-11-23 Created: 2015-11-23 Last updated: 2017-10-18Bibliographically approved
In thesis
1. Packed Column Supercritical Fluid Chromatography: Applications in Environmental Chemistry
Open this publication in new window or tab >>Packed Column Supercritical Fluid Chromatography: Applications in Environmental Chemistry
2017 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Although gas and liquid chromatography have emerged as dominant separation techniques in environmental analytical chemistry, these methods do not allow for the concurrent analysis of chemically diverse groups of persistent organic pollutants (POPs). There are also a small number of compounds which are not easily amenable to either of these traditional separation techniques. The main objective of this thesis was to address these issues by demonstrating the applicability of packed column supercritical fluid chromatography (pSFC) coupled to mass spectrometry (MS) in various aspects of environmental chemistry.

First, pSFC/MS analytical methods were developed for legacy POPs (PCDDs, PCDFs, and PCBs) as well as the emerging environmental contaminant Dechlorane Plus (DP), and issues relating to the ionization of target analytes when pSFC was coupled to MS were explored. Novel APPI and APCI reagents (fluorobenzene and triethylamine) were optimized and real samples (water and soil) were analyzed to demonstrate environmental applicability.

The possibility of chiral and preparative scale pSFC separations was then demonstrated through the isolation and characterization of thermally labile hexabromocyclododecane (HBCDD) stereoisomers. The analytical pSFC separation of the α-, β-, and γ-HBCDD enantiomers as well as the δ and ε meso forms was shown to be superior to results obtained using a published LC method.

Finally, technical mixtures of phosphorus flame retardants (RBDPP, BPA-BDPP, and DOPO; a group of related compounds which are challenging to analyze concurrently) were examined using multiple analytical techniques and pSFC was found to be the only method which facilitated the accurate determination of the components of all 3 mixtures. This thesis confirms the potential of pSFC/MS as a fast, green, and cost effective means of separating and analyzing environmental contaminants.

Place, publisher, year, edition, pages
Örebro: Örebro University, 2017. 87 p.
Series
Örebro Studies in Chemistry, ISSN 1651-4270 ; 19
Keyword
Supercritical Fluid Chromatography, Mass Spectrometry, Ionization, POPs, APPI, APCI, chiral, achiral, packed column
National Category
Other Chemistry Topics
Identifiers
urn:nbn:se:oru:diva-56826 (URN)978-91-7529-184-0 (ISBN)
Public defence
2017-05-12, Örebro universitet, Billbergska huset, Hörsal B, Fakultetsgatan 1, Örebro, 10:15 (English)
Opponent
Supervisors
Available from: 2017-03-27 Created: 2017-03-27 Last updated: 2017-10-18Bibliographically approved

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