Publication Abstract

The performance characteristics of a method involving liquid chromatography electrospray ionisation tandem mass spectrometry method for the determination of organophosphorus flame retardants and plasticisers in marine sediments and surface waters have been established. The approach permits the determination of thirteen compounds including three alkyl phosphates, two aryl phosphates, chlorinated alkyl phosphates/phosphite, synthetic intermediates and non-derived alkyl phosphates. Marine sediments were extracted using accelerated solvent extraction followed by gel permeation chromatography clean-up and the resulting extracts required no further clean-up prior to analysis. The recoveries of selected determinants ranged between 71 and 112 % with relative standard deviations between 4 and 23 %. Analytes were also isolated from surface water samples using solid phase extraction. This method provided recoveries of between 71 and 117 % and relative standard deviations of between 3 and 18 %. The recoveries of trimethyl phosphate were found to be poor and the compound was thus excluded from all subsequent determinations. Separation of analytes was achieved using a C18 analytical column and mass spectral data were obtained using an ion trap mass spectrometer operated in positive electrospray ionisation mode. Analytical limits of quantification ranged between 1 to 10 ng/L for surface waters and from 1 to 11 ng/g dry weight for marine sediment, making the method suitable for trace level environmental analysis. A limited survey conducted on thirteen marine and three riverine sediment samples revealed the presence of eight organophosphorus compounds at concentrations ranging from 1.2 ng/g to 179 ng/g