PMID- 29937123 OWN - NLM STAT- MEDLINE DCOM- 20180813 LR - 20181202 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1565 DP - 2018 Aug 31 TI - Thorough study of persistent organic pollutants and halogenated natural products in sperm whale blubber through preparative sample cleanup followed by fractionation with countercurrent chromatography. PG - 114-123 LID - S0021-9673(18)30793-3 [pii] LID - 10.1016/j.chroma.2018.06.037 [doi] AB - Marine mammals are top predators of the marine food chain and thus known to bioaccumulate high concentrations of polyhalogenated compounds. Yet, details of the organohalogen pattern are largely unknown. For this reason, we isolated the polyhalogenated compounds from 750 g blubber of a sperm whale (Physeter catodon), which deceased at the German North Sea coast in January 2016. The sample matrix was decomposed by sulfuric acid treatment and the polyhalogenated compounds were then fractionated by countercurrent chromatography (CCC). Seventy-three CCC fractions were taken and analyzed by gas chromatography with electron capture negative ion mass spectrometry (GC/ECNI-MS). The bulk of the polyhalogenated compounds in the sample originated from classic persistent organic pollutants (POPs). Altogether 90 polychlorinated biphenyl (PCB) congeners were detected in the sample including all possible octa- to decachloro congeners except one. The sample also featured 105 toxaphene congeners including 30 chlorobornenes (contribution approximately 14% of the total toxaphene content) which were only detected after the CCC fractionation. In addition, several chlordane and mirex related compounds were detected which were never or very scarcely described before in biota. Classic POPs (PCBs, DDT, toxaphene, chlordane, mirex) were predominant, while new emerging contaminants were scarcely detected. The sample featured several halogenated natural products (HNPs) some of which were less stable and destroyed during the sample cleanup involving treatment with sulfuric acid. Sample fractionation by means of CCC was crucial for the detection and assignment of many of the uncommon polyhalogenated compounds. CI - Copyright (c) 2018 Elsevier B.V. All rights reserved. FAU - Vetter, Walter AU - Vetter W AD - University of Hohenheim, Institute of Food Chemistry (170b), Garbenstrasse 28, D-70599 Stuttgart, Germany. Electronic address: walter.vetter@uni-hohenheim.de. FAU - Lok, Bianca AU - Lok B AD - University of Hohenheim, Institute of Food Chemistry (170b), Garbenstrasse 28, D-70599 Stuttgart, Germany. FAU - Schlienz, Annika AU - Schlienz A AD - University of Hohenheim, Institute of Food Chemistry (170b), Garbenstrasse 28, D-70599 Stuttgart, Germany. FAU - Muller, Marco AU - Muller M AD - University of Hohenheim, Institute of Food Chemistry (170b), Garbenstrasse 28, D-70599 Stuttgart, Germany. LA - eng PT - Journal Article DEP - 20180619 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Biological Products) RN - 0 (Organic Chemicals) RN - 0 (Water Pollutants, Chemical) RN - 8001-35-2 (Toxaphene) RN - DFC2HB4I0K (Polychlorinated Biphenyls) SB - IM MH - Adipose Tissue/chemistry MH - Animal Structures/*metabolism MH - Animals MH - Biological Products/*analysis MH - Chemical Fractionation MH - Countercurrent Distribution/*methods MH - *Environmental Monitoring MH - Gas Chromatography-Mass Spectrometry MH - *Halogenation MH - Human Activities MH - Humans MH - Male MH - Organic Chemicals/*analysis MH - Polychlorinated Biphenyls/analysis MH - Sperm Whale/*anatomy & histology MH - Toxaphene/analysis MH - Water Pollutants, Chemical/*analysis OTO - NOTNLM OT - Countercurrent chromatography OT - GC/MS OT - Halogenated natural products OT - Marine mammals OT - Persistent organic pollutants EDAT- 2018/06/26 06:00 MHDA- 2018/08/14 06:00 CRDT- 2018/06/26 06:00 PHST- 2018/02/28 00:00 [received] PHST- 2018/06/11 00:00 [revised] PHST- 2018/06/16 00:00 [accepted] PHST- 2018/06/26 06:00 [pubmed] PHST- 2018/08/14 06:00 [medline] PHST- 2018/06/26 06:00 [entrez] AID - S0021-9673(18)30793-3 [pii] AID - 10.1016/j.chroma.2018.06.037 [doi] PST - ppublish SO - J Chromatogr A. 2018 Aug 31;1565:114-123. doi: 10.1016/j.chroma.2018.06.037. Epub 2018 Jun 19.