Shape-selective extraction of PCBs and dioxins from fish and fish oil using in-cell carbon fractionation pressurized liquid extraction.
This paper describes a new shape-selective, pressurized liquid extraction (PLE) procedure for extracting polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) and PCBs from food and feed samples with an integrated carbon fractionation step. Initially this was done using specially designed inserts for 34-mL cells, but subsequently, large solid cells (66 mL) were machined to increase the capacity and robustness of the system. Depending on the carbon load and extraction solvent strength, the non-ortho PCBs were recovered either with the bulk of the PCBs or with the PCDD/Fs. The former is preferable if PCDD/Fs are the targets. In most cases, however, data are required for all indicator PCBs, WHO-PCBs, and PCDD/Fs. Therefore, further efforts focused on developing, optimizing, and validating a cost- and time-efficient PLE procedure that can extract these targets, separate non-ortho PCBs and PCDD/Fs from the bulk of the PCBs, allow gravimetric fat determinations, and requires a minimum of postextraction cleanup. The performance of the resulting procedure was assessed in experiments with a fish tissue reference material. The trueness of the WHO-PCB-TEQ, PCDD/F-TEQ, and total-TEQ data were -8, -5, and -7%, respectively, and the corresponding CVs were 1.5, 0.5, and 1.3%; within the limits set by the European community for gas chromatography-high-resolution mass spectrometry methods for food and feed control.
Haglund
P
P
Department of Chemistry, Umeå University, S-901 87 Umeå, Sweden. peter.haglund@chem.umu.se
Sporring
S
S
Wiberg
K
K
Björklund
E
E
D000818:Animals; D001572:Benzofurans / Q000032:analysis*; D002244:Carbon / Q000737:chemistry*; D002853:Chromatography, Liquid / Q000379:methods; D004867:Equipment Design; D005395:Fish Oils / Q000737:chemistry*; D005399:Fishes; D008401:Gas Chromatography-Mass Spectrometry / Q000295:instrumentation / Q000379:methods; D010316:Particle Size; D011078:Polychlorinated Biphenyls / Q000032:analysis*; D000072317:Polychlorinated Dibenzodioxins / Q000031:analogs & derivatives* / Q000032:analysis; D012680:Sensitivity and Specificity
D001572:Benzofurans; D005395:Fish Oils; D000072317:Polychlorinated Dibenzodioxins; D002244:Carbon; C023614:dibenzofuran; D011078:Polychlorinated Biphenyls