A method for the analysis of multiple novel halogenated flame retardants in cow's milk.
A method was developed for the extraction and analysis of cow's milk to measure 21 halogenated flame retardants (FRs), including individual isomers plus eight methoxy-polybrominated diphenyl ethers (MeO-PBDEs). Extraction was performed using homogenisation with acetone:hexane with size exclusion chromatography followed by adsorption chromatography clean-up. Analysis was undertaken using gas chromatography high-resolution mass spectrometry. The method was validated in fortified cow's milk with FRs and 2-methoxy-PBDE 68 at three levels (low [12.5-1250 pg g(-)(1)], mid [37.5-5000 pg g(-)(1)] and high [400-10 000 pg g(-)(1)]). Additional methoxy-PBDEs were tested at two fortification levels. Isotope dilution was used to correct for losses during sample preparation and average recoveries ranged from 58% (allyl 2,4,6-tribromophenyl ether [ATE]) to 121% (γ-tetrabromoethylcyclohexane (γ-TBECH)). Limits of detection ranged from 0.055 pg g(-)(1) (6-methoxy-PBDE 47) to 38.9 pg g(-)(1) (decabromodiphenylethane (DBDPE)). Matrix effects were overcome through the use of surrogate and performance standards. A single FR (1-bromomethyl-2,3,4,5,6-pentabromobenzene [PBBB]) and two methoxy-PBDEs were detected in commercially available cow's milk collected from local supermarkets in Ottawa, ON, Canada. Detection frequency was < 25% for these compounds and, where present, concentrations were low.
a Food Research Division, Bureau of Chemical Safety, Health Products and Food Branch , Health Canada , Ottawa , ON , Canada.
Dorothea F K
DF
Rawn
a Food Research Division, Bureau of Chemical Safety, Health Products and Food Branch , Health Canada , Ottawa , ON , Canada.
Catherine
C
Corrigan
a Food Research Division, Bureau of Chemical Safety, Health Products and Food Branch , Health Canada , Ottawa , ON , Canada.
Cathie
C
Ménard
a Food Research Division, Bureau of Chemical Safety, Health Products and Food Branch , Health Canada , Ottawa , ON , Canada.
François
F
Breton
a Food Research Division, Bureau of Chemical Safety, Health Products and Food Branch , Health Canada , Ottawa , ON , Canada.
Wing-Fung
WF
Sun
D000818:Animals; D004784:Environmental Monitoring; D004785:Environmental Pollutants / Q000032:analysis*; D005411:Flame Retardants / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods* / Q000592:standards; D055768:Halogenated Diphenyl Ethers / Q000032:analysis*; D006801:Humans; D057230:Limit of Detection; D059625:Liquid-Liquid Extraction / Q000379:methods; D008892:Milk / Q000737:chemistry*; D011075:Polybrominated Biphenyls / Q000032:analysis*
D004785:Environmental Pollutants; D005411:Flame Retardants; D055768:Halogenated Diphenyl Ethers; D011075:Polybrominated Biphenyls
GC-HRMS; Novel flame retardants; analysis; cow’s milk