Validation of a Cleanup Method for Analysis of Novel Brominated Flame Retardants in Biota Matrices Sofie Björklund 2015-05-30 Supervisors Ingrid Ericson

Sammanfattning: Brominated flame retardants is a group of compounds present in numerous types of materials in our surroundings. Although their purpose is to slow the progression of a fire, many has been shown to be toxic to the environment. Novel brominated flame retardants have been introduced to the market as old ones have been removed. Reliable methods are crucial to be able to monitor how the novel brominated flame retardant spread and accumulate in the environment. To achieve this, a method validation of a cleanup method using multilayer silica followed by analysis by atmospheric pressure gas chromatography coupled to tandem mass spectroscopy was performed. This method had been previously used for polybrominated diphenyl ethers and the aim was to see if it could be used for analysis of novel brominated flame retardants as well. Spiking experiments showed generally good results, with recoveries of the native compound ranging from 40% to 174%. To apply the method on real matrix samples, eight samples of osprey eggs and five samples of adipose tissue of ringed seal was analyzed. Several novel brominated flame retardants were found, most abundant being the methoxylated polybrominated diphenyl ethers. Dominant congener was 2'-Methoxy-2,3',4,5'-tetrabromodiphenyl ether (2PMBDE#68) followed by 6-Methoxy-2,2',4,4'-tetrabromodiphenyl ether (6PMBDE#47), 5-Methoxy-2,2',4,4'-tetrabromodiphenyl ether (5PMBDE#47) and 5-Methoxy-2,2',4,4',6-pentabromodiphenyl ether (5PMBDE#100) with concentrations ranging from <0,13-13 ng/g lipid weight in osprey eggs and <0,003-249 ng/g lipid weight in ringed seal blubber. Also 1,2-Bis(2,4,6-tribromophenoxy)ethane and pentabromobenzene were found in both osprey eggs and ringed seal blubber. Hexabromobenzene was found in ringed seal blubber and 2,3,5,6-tetrabromo-p-xylene was identified in osprey eggs.