Premium
Analysis of organochlorines in harbor seal ( Phoca vitulina ) tissue samples from Alaska using gas chromatography/ion trap mass spectrometry by an isotopic dilution technique
Author(s) -
Wang Dongli,
Atkinson Shan,
HooverMiller Anne,
Li Qing X.
Publication year - 2005
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.1990
Subject(s) - phoca , chemistry , chromatography , gas chromatography , mass spectrometry , detection limit , harbor seal , fraction (chemistry) , isotope dilution , gas chromatography–mass spectrometry , environmental chemistry , fishery , biology
A gas chromatography/ion trap mass spectrometry (GC/ITMS) method was developed for the determination of organochlorine pesticides (OCPs), polychlorinated biphenyls (PCBs) and polychlorinated naphthalenes (PCNs) in harbor seal ( Phoca vitulina ) tissues. Tissue samples were homogenized, lyophilized and fortified with 13 C‐PCBs 28, 123, 169 and 170, and then extracted with an accelerated solvent extractor with a mixture of hexane and methylene chloride (1:1, v/v). After lipid removal using a 40% H 2 SO 4 ‐modified silica gel column, all organochlorines were collected in one fraction and further fractionated with an activated carbon/silica gel (1:20) column into a first fraction containing OCPs, non‐coplanar PCBs and 13 C‐PCBs 28, 123 and 170, and a second containing PCNs, coplanar PCBs and 13 C‐PCB 169. Prior to GC/MS/MS analysis, 13 C‐PCB 169 was added into the first fraction as an injection standard and 13 C‐PCB 170 into the second fraction to calibrate the recoveries of the fortified internal standards. This method can effectively eliminate matrix interferences, and has high selectivity and sensitivity. Recoveries averaged 45–86% for OCPs with relative standard deviations (RSDs) of 2–14%, 52–137% for PCBs with RSDs of 3–29% and 36–152% for PCNs with RSDs of 7–29% from lard and chicken heart samples, which were used as alternative matrices to harbor seal samples in recovery studies. The limits of detection for OCPs, PCBs and PCNs were 0.7–1.9, 1.5–8.9 and 0.5–10 pg/g dry weight, respectively. This method can be used to analyze OCPs, PCBs and PCNs in harbor seal blubber, liver and kidney samples. Copyright © 2005 John Wiley & Sons, Ltd.