Analysis of Hexabromocyclododecane (HBCDD) in Environmental Samples by Liquid Chromatography Mass Spectrometry

Hexabromocyclododecane (HBCDD) is a brominated flame retardant that has been identified as a priority substance within the European Water Framework Directive and must be monitored in the environment by regulatory bodies such as Natural Resources Wales. This project investigated the extraction and analysis of the three main isomers of HBCDD in different matrices including freshwater, saline and biota, exploring different compound extraction techniques to find the optimal procedure for each matrix investigated and finding the optimal parameters for analysis. A method for analysis of aqueous saline and freshwater matrices was developed and validated involving an extraction procedure using hydrophilic-lipophilic balance (HLB) solid phase extraction (SPE) disks, elution into methanol and a x1000 concentration of the sample extract. Analysis was conducted via liquid chromatography tandem mass spectrometry with a quadrupole mass spectrometer operating in negative electrospray ionisation mode. The target limit of quantitation values for each isomer of 75 pg/L and 150 pg/L for saline and freshwater matrices respectively was achieved in both matrices, with % accuracies for both matrices ranging from 97.3 – 102.7% and every isomer in both saline and freshwater fell below the precision target of <15% RSD. Initial method development on biota matrix involved research of QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) kits with alternative dispersive SPE kits tested, and investigation into homogenisation techniques of the biota matrix. The result of this project was implementation of a fully validated method for extraction and analysis of HBCDD in saline and freshwater matrices as a routine monitoring test of HBCDD abundance in the environment. Further work will need to be conducted on the analysis of HBCDD in biota matrix