Comparison of in-cell lipid removal efficiency of adsorbent mixtures for extraction of polybrominated diphenyl ethers...

Polybrominated diphenyl ethers (PBDEs) have become ubiquitous environmental contaminants due to their incorporation into many consumer products. Their ability to bioaccumulate to alarming levels in fat-rich matrices such as fish demands fast and efficient methods to monitor these contaminants. We present an analytical method for selective-pressurised liquid extraction (S-PLE) of PBDEs from fish tissue. Fat removal performance of different mixtures of Florisil, silica gel and sulphuric acid-impregnated silica gel were evaluated using a response surface experimental design approach for determining the optimal fat-retaining mixture for S-PLE. Acid-silica gel had the greatest individual effect on fat retention; with a two-thirds acid-silica one-third Florisil mixture found to be the most efficient (>97%). Method validation was performed using recovery experiments at three spiked concentration levels (0.05, 0.5 and 5ngg(-1) ww). Mean recoveries of target analytes in spiked samples ranged from 70 to 124%, with relative standard deviations <27%. The S-PLE lipid removal efficiency combined with the sensitivity of triple quadrupole mass spectrometers provides a fast and comparatively inexpensive analytical method for analysis of PBDEs in fish samples.