title: An efficient clean-up method for the GC-MS determination of methylsulfonyl-PCBs/DDEs extracted from various marine mammal tissues.
abstract: Existing methods for analyzing methylsulfonyl-PCBs in animal tissues require multiple laborious clean-up steps prior to quantitation. In this paper, we report a new, efficient method for the isolation and determination of methylsulfonyl-PCB metabolites in the blubber, liver, kidney, lung, and milk from mammals of marine origin using: solvent extraction, GPC fractionation, and clean-up on an adsorption chromatography column prior to analysis by gas chromatography-mass spectrometry. The method is rapid and can be completed in about half the analysis time required by most other reported methods. The method exhibits excellent analyte recoveries (89-95%), and good reproducibilities with CV's ranging from 3-12% depending on analyte concentration. Detection limits are approximately 1 ng/g lipid. The method is further validated by comparing its quantitative results to that of an independent reference analytical method for several different marine mammal blubber samples. Finally, the method is applied to profile the distribution of methylsulfones among the various tissue types studied for a single bottle-nose dolphin (Tursiops truncatus) sample. In addition, the extent of their transplacental transfer from mother to unborn fetus for several pilot whale (Globicephala melaena) mother-fetus pairs is examined.
authors.affiliation: Environmental Conservation Division, Northwest Fisheries Science Center, National Marine Fisheries Service, National Oceanic & Atmospheric Administration, Seattle, WA 98112, USA. david.herman@noaa.gov
authors.forename: D P
authors.initials: DP
authors.lastname: Herman
authors.forename: J I
authors.initials: JI
authors.lastname: Effler
authors.forename: D T
authors.initials: DT
authors.lastname: Boyd
authors.forename: M M
authors.initials: MM
authors.lastname: Krahn
mesh_terms: D000273:Adipose Tissue / Q000737:chemistry; D000327:Adsorption; D000818:Animals; D002845:Chromatography / Q000379:methods; D003633:Dichlorodiphenyl Dichloroethylene / Q000032:analysis* / Q000493:pharmacokinetics; D004784:Environmental Monitoring / Q000379:methods*; D004785:Environmental Pollutants / Q000032:analysis* / Q000493:pharmacokinetics; D005260:Female; D008401:Gas Chromatography-Mass Spectrometry; D007306:Insecticides / Q000032:analysis* / Q000493:pharmacokinetics; D008297:Male; D008322:Mammals; D008431:Maternal-Fetal Exchange; D011078:Polychlorinated Biphenyls / Q000032:analysis* / Q000493:pharmacokinetics; D011247:Pregnancy; D012680:Sensitivity and Specificity; D014018:Tissue Distribution; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000493:pharmacokinetics
chemical_list: D004785:Environmental Pollutants; D007306:Insecticides; D014874:Water Pollutants, Chemical; D003633:Dichlorodiphenyl Dichloroethylene; D011078:Polychlorinated Biphenyls