Automated pressurized liquid extraction (PLE) and automated power-prep (TM) clean-up for the analysis of polycyclic aromatic hydrocarbons, organo-chlorinated pesticides and polychlorinated biphenyls in marine samples

作者：Helaleh Murad I H^*; Al Rashdan Amal

来源：Analytical Methods, 2013, 5(6): 1617-1622.

DOI：10.1039/c3ay26428a

An accurate and precise analytical method for the determination of polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs), and organo-chlorinated pesticides (OCPs) in fish and shellfish based on automated pressurized liquid extraction (PLE) and automated power-prep (TM) clean-up has been developed. After extraction, the extract was passed through gel permeation chromatography (GPC) using 12 g of Bio-beads SX-3 for fat removal. GC/MS (NCI) was selected for OCPs and PCBs due to its high sensitivity and selectivity of NCI to chlorinated compounds and GC/MS (EI) for PAHs. The method was validated using spiked surrogates of C-13-PCBs, deuterated PAH (d-PAHs) and fish reference material (EDF-2525). All of the recoveries are within the acceptance levels and in accordance with the US-EPA standard methods. The calibration ranges for most of the compounds were from 50 to 1000 ng ml(-1) for PAHs, 10 to 103 ng ml(-1) for PCBs and 10 to 200 ng ml(-1) for OCPs. The limits of detection ranged between 0.01 and 0.28 ng g(-1) (w/w) for PCBs, 0.03-2.48 ng g(-1) (w/w) for OCPs and 0.1 to 1.0 ng g(-1) (w/w) for PAHs. Analytical criteria, such as repeatability and reproducibility were evaluated through a range of biological matrices and fish reference material analysis. The feasibility of extraction using a power-prep (TM)/PLE system combined with power-prep (TM) automated clean-up demonstrated a validated method for the analysis of biota samples.

• 出版日期2013