Establishing the occurrence and profile of polycyclic aromatic hydrocarbons in marine sediments: The eastern Mediterranean coast of Spain as a case study.

Sampling, cost-effective analysis, diagnosis of sources of pollution and assessment of potential toxicological effects were included in the case study. Marine sediments collected from 24 points along the eastern Mediterranean coast of Spain (Comunitat Valenciana region) in 2010, 2011, 2012 and 2015 have been analysed for polycyclic aromatic hydrocarbons. Fluoranthene, pyrene, chrysene, benzo[b]fluoranthene and benzo[a]pyrene were the most found. An analysis of the relative abundance of selected PAHs revealed that petrogenic and mixed petrogenic/pyrogenic sources are predominant in the area. The total concentrations of the target compounds ranged from 14.7 to 615.3 ng/g dry weight. The effects range-low (ERL) guideline values were used to assess potential toxicological effects. Rarely adverse biological effects can be expected in the tested area. The level of pollution by PAHs in the area can be considered low, although occasionally high values can be found, particularly in areas with high population or ship traffic.

Improving detection limits for organotin compounds in several matrix water samples by derivatization-headspace-solid-phase microextraction and GC-MS.

Triethyltin, tributyltin, diphenyltin and triphenyltin were selected as model compounds. The method is based on in situ ethylation and simultaneous headspace-solid-phase microextraction (HS-SPME) and gas chromatographic-mass spectrometry analysis (GC-MS). The extraction procedure was optimized studying some variables such as reaction time, salinity, sample volume and headspace volume. SPME-GC-MS and SPME-GC-FID techniques were compared; quality assurance parameters such as sensitivity, selectivity and precision were established. The proposed procedure showed limits of detection between 0.025 and 1ng/L. The linearity was in the 0.025-5000 ng/L range. The precision expressed as relative standard deviations (RSD), were below 20%. Real wastewaters and seawaters were analyzed. The method permits controlling legislated annual average values.

Miniaturized matrix solid phase dispersion procedure and solid phase microextraction for the analysis of organochlorinated pesticides and polybrominated diphenylethers in biota samples by gas chromatography electron capture detection.

This work has developed a miniaturized method based on matrix solid phase dispersion (MSPD) using C18 as dispersant and acetonitrile-water as eluting solvent for the analysis of legislated organochlorinated pesticides (OCPs) and polybrominated diphenylethers (PBDEs) in biota samples by GC with electron capture (GC-ECD). The method has compared Florisil-acidic Silica and C18 as dispersant for samples as well as different solvents. Recovery studies showed that the combination of C18-Florisil was better when using low amount of samples (0.1 g) and with low volumes of acetonitrile-water (2.6 mL). The use of SPME for extracting the analytes from the solvent mixture before the injection resulted in detection limits between 0.3 and 7.0 microg kg(-1) (expressed as wet mass). The miniaturized procedure was easier, faster, less time consuming than the conventional procedure and reduces the amounts of sample, dispersant and solvent volume by approximately 10 times. The proposed procedure was applied to analyse several biota samples from different parts of the Comunidad Valenciana.