Congener-specific method for the determination of ortho and non-ortho polychlorinated biphenyls, polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans in foods by carbon-column fractionation and gas chromatography-isotope dilution mass spectrometry

Krokos, F.; Creaser, Colin S.; Wright, Christopher I.; Startin, James R.

doi:10.1007/s002160050240

Cited by 23 publications

(11 citation statements)

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“…The use of a carbon column has previously been demonstrated to be suitable for the separation of ortho-substituted PCB, non-ortho substituted PCB, and PCDD/F according to their structure-affinity relationship [20]. In this study, however, only the cPCB were actually isolated via the carbon column, because their coplanar 376 properties enable them to be trapped between planar carbon layers until their displacement by use of the structurally related toluene solvent [21].…”

Section: Correlation Of the Retention Of Pcb With Their Electronic Anmentioning

confidence: 98%

An improved clean-up strategy for simultaneous analysis of polychlorinated dibenzo-p-dioxins (PCDD), polychlorinated dibenzofurans (PCDF), and polychlorinated biphenyls (PCB) in fatty food samples

2002

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The study and extension of a simple automated clean-up method for polychlorinated dibenzo-p-dioxins (PCDD) and polychlorinated dibenzofurans (PCDF) to a broad range of polychlorinated biphenyls (PCB) is described. The isolation of seven PCDD, ten PCDF, and three coplanar PCB (cPCB) is extended to eight monoortho substituted PCB and seven so-called "marker PCB" (Aroclor 1260) for fatty food samples. This enables quantification of 35 compounds - including all congeners with a WHO toxic equivalent factor (TEF)--in a single extraction and single purification step. The chromatographic behaviour of mono-ortho PCB and marker PCB on a variety of adsorbents, including basic alumina, has been studied. Partitioning of analytes through multi-column sequences is described and correlated with their structural and electronic properties, by use of molecular modelling calculations. The fractionation process available with the Power-Prep automated clean-up system enables rapid independent analysis of the different groups of compounds. Gas chromatography with high resolution mass spectrometry (GC-HRMS) is used for the PCDD/F and cPCB fraction and quadrupole ion-storage tandem in time mass spectrometry (GC-QISTMS) for analysis of the remaining PCB. A comparison study was performed on quality-control samples and real fatty food samples to evaluate the robustness of the new strategy compared with a reference method. On the basis of this simultaneous clean-up, a rapid simplified strategy for PCDD/F and selected PCB analysis determination is proposed for fatty food samples.

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Section: Correlation Of the Retention Of Pcb With Their Electronic Anmentioning

confidence: 98%

An improved clean-up strategy for simultaneous analysis of polychlorinated dibenzo-p-dioxins (PCDD), polychlorinated dibenzofurans (PCDF), and polychlorinated biphenyls (PCB) in fatty food samples

2002

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“…Extraction and cleanup were performed by matrix solid phase dispersion following a semiautomatic procedure [17] previously described in detail [16]. This comprises a low‐pressure liquid chromatography system in which the three non‐ ortho (77, 126, and 169) PCBs (Fraction A) were separated from the bulk of the PCBs and lipids (Fraction B).…”

Section: Methodsmentioning

confidence: 99%

“…Gas chromatographic separation of the nine atropisomeric PCB congeners in their atropisomers was carried out with the Thermo Quest Finnigan HRGC/ITD system described previously, using a Chirasil‐Dex column (25 m × 0.25‐mm i.d., 0.2‐μm film thickness, Alltech, Deerfield, IL, USA) [17].…”

Section: Methodsmentioning

confidence: 99%

Isomer‐specific polychlorinated biphenyl determination in cetaceans from the mediterranean sea: Enantioselective occurrence of chiral polychlorinated biphenyl congeners

Jiménez

Jiménez²,

González³

2000

Enviro Toxic and Chemistry

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Isomer-specific concentrations of 41 polychlorinated biphenyls (PCBs) and the enantiomeric ratios (ER) of nine chiral PCBs were determined in the liver of four cetacean species-Risso's dolphin (Grampus griseus), bottlenose dolphin (Tursiops truncatus), fin whale (Balaenoptera physalus), and long-finned pilot whale (Globicephala melaena)-found dead in the Mediterranean Sea. The total PCB concentration (sum of 41 congeners) ranged from 484 to 63,200 ng/g wet weight. The 2,3,7,8 tetrachlorodibenzo-p-dioxin (TCDD) toxic equivalents (TEQs), as defined by the World Health Organization (WHO), ranged from 4.3 to 1,454 pg/g wet weight. The contribution of mono-ortho PCBs was consistently higher than non-ortho PCB congeners, in whale species, whereas in dolphins this predominance was not so clear. The PCB profiles were dominated by congeners 138, 153, and 180 in almost all the investigated samples. Comparison of PCB profiles by using principal component analysis allowed to separate the species into different groups. Polychlorinated biphenyls 170 and 180 seem to be eliminated by the two whale species, and PCB 180 also seems to be eliminated by Risso's dolphins. The PCBs 95, 132, 149, and 176 revealed an enantiomeric excess of the second eluted enantiomer in almost all the cetaceans investigated, where 136 and 174 were racemic or almost racemic. It is the first time that an enantiomeric excess of PCB 84 and 91 has been reported in biological samples. Although it was only possible to calculate them in two dolphin liver samples, the high values of enantiomeric excess found are surprising (86.3 and 32% for PCB 91 and 84, respectively).

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“…Silica and alumina or Florisil are used to fractionate or remove as many non-dioxin-like compounds as possible prior to the carbon cleanup stage. Poole et al (1990), Krokos et al (1997), Kloskowski et al (2007), Fernandez et al (2004), Djien Liem, (1999), Sandra, Frank and Vanhoenecker (2008), Santos and Galceran (2002) have reviewed a variety of sample preparation techniques for gas chromatographic analysis.…”

Section: Extract Cleanupmentioning

confidence: 99%

The analysis of dioxins and related compounds

Reiner

2009

Mass Spectrometry Reviews

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The analysis of polychlorinated dibenzo-p-dioxins, polychlorinated dibenzofurans, polychlorinated biphenyls, and other related compounds requires complex sample preparation and analytical procedures using highly sensitive and selective state-of-the-art instrumentation to meet very stringent data quality objectives. The analytical procedures (extraction, sample preparation), instrumentation (chromatographic separation and detection by mass spectrometry) and screening techniques for the determination of dioxins, furans, dioxin-like polychlorinated biphenyls and related compounds with a focus on new approaches and alternate techniques to standard regulatory methods are reviewed.

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Congener-specific method for the determination of ortho and non-ortho polychlorinated biphenyls, polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans in foods by carbon-column fractionation and gas chromatography-isotope dilution mass spectrometry

Cited by 23 publications

References 0 publications

An improved clean-up strategy for simultaneous analysis of polychlorinated dibenzo-p-dioxins (PCDD), polychlorinated dibenzofurans (PCDF), and polychlorinated biphenyls (PCB) in fatty food samples

An improved clean-up strategy for simultaneous analysis of polychlorinated dibenzo-p-dioxins (PCDD), polychlorinated dibenzofurans (PCDF), and polychlorinated biphenyls (PCB) in fatty food samples

Isomer‐specific polychlorinated biphenyl determination in cetaceans from the mediterranean sea: Enantioselective occurrence of chiral polychlorinated biphenyl congeners

The analysis of dioxins and related compounds

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