Automated Determination of Xenobiotics (Pesticides, PCBs, PAHs, and PBDEs) in Sediment Samples Applying HS-SPME-GC-HRMS

Background: Automated methods are needed for the reliable determination of xenobiotics in environmental samples. Objective: Optimization and application of an automated method for the ultra-trace analysis of 34 organic contaminants including polycyclic aromatic hydrocarbons (PAHs), polybrominated diphenyl ethers (PBDEs), polychlorinated biphenyls (PCBs), organochlorinated (OCPs), and organophosphorus pesticides (OPPs) in sediment samples have been performed. Methods: Automated method based on headspace solid-phase microextraction (SPME) coupled to GC high-resolution MS (GC-HRMS) for the ultra-trace analysis of the targeted compounds has been developed. Conclusions: Suitable validation parameters in terms of linearity, trueness, selectivity, intraday and interday precision, LODs, and LOQs were obtained. Relative recovery values between 70 and 120% were achieved for all compounds (concentration levels assayed 1 and 10 mu g/kg). RSD values were always lower than 25% for intra- and interday precision, and LODs and LOQs were 0.1 and 1.0 mu g/kg, respectively, for all analytes. Highlights: The proposed method was applied to the analysis of sediments collected in Andalusia, Spain, and Poland, finding PCB 18 in one sample (15.9 mu g/kg) and p,p'-DDE in several samples at concentrations ranging from 27.6 to 297.2 mu g/kg.