Analytical method for the determination of halogenated norbornene flame retardants in environmental and biota matrices by gas chromatography coupled to tandem mass spectrometry

A new methodology for the analysis of Dechlorane Plus and related compounds (DPMA, Dec 602, Dec 603 and Dec 604) by gas chromatography coupled to negative chemical ionization tandem mass spectrometry (GC–NCI–MS–MS) was developed for three different matrices, including environmental (sediment and sludge) and biota (fish) samples. Analytical parameters such as linearity, repeatability and reproducibility, recoveries, limits of detection and limits of quantification were evaluated, showing satisfactory values for the developed methodology. Moreover, a comparison with the analysis by GC–NCI–MS was carried out. Method limits of detection (MDLs), ranging between 0.12 and 1.26 pg/g dw, 1.16–2.90 pg/g dw and 2.30–21.1 pg/g lw for sediment, sludge and fish respectively, were much better than those obtained by GC–MS, with improvement factor up to 320. The applicability of the developed methodology was demonstrated by the analysis of real samples collected in a non-producing area, the Ebro river basin (Spain). DP values were up to 1.61 ng/g dw, 18.8 ng/g dw and 2.24 ng/g lw for sediment, sludge and fish samples, respectively.