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Although restricting environmental quality values for organotin compounds (OTs) are set by Directive 2013/39/EU of the European Parliament, marine environment remains being affected due to maritime circulation at global scale. Fish and seafood accumulate OTs, making fish and seafood consumption the main source of OTs in humans. Because of the fish and seafood matrices complexity and the required low limits of detection, a robust and fast procedure for the quantification of OTs in fish and seafood, using ultrasound-assisted extraction and gas chromatography–tandem mass spectrometry, was validated and applied. Detection (2.7 µg Sn kg−1) and quantification (8.0 µg Sn kg−1) limits, repeatability and intermediate precision (<10%), accuracy by analysing ERM®-CE477 Mussel Tissue and analytical recoveries (65–122%) were assessed. Multivariate analysis shown that the matrix effect for some OTs displayed good negative correlation with the fat and protein content. Health risk assessment of OTs intake revealed no serious risk for human consumption. [ABSTRACT FROM AUTHOR]

A simple, effective, and economic method for determination of nine triazines (ametryn, atrazine, cyanazine, prometryn, propazine, simazine, simetryn, terbuthylazine, and terbutryn) in drinking water based on solid-phase extraction (SPE) followed by high-performance liquid chromatography-diode array detection (HPLC-DAD) was developed. A specialized solid phase (Oasis HLB) was used, and the parameters that may affect the efficiency of SPE were optimized. The limits of detection (ranged from 0.010 to 0.023 µg L−1) were satisfactory and allow the determination of triazines at the levels required by European Union legislation. Repeatability (2.4–7.6%) and intermediate precision (0.9–11.0%) calculated at 0.1 µg L−1(legislation level) were adequate. The accuracy calculated as the average recovery of spiked tap and mineral waters was higher than 86% for all compounds. The developed method also could be used for undergraduate laboratory experiments because it acquaints students with solution preparation, solid phase extraction procedure, and HPLC-DAD technique. [ABSTRACT FROM PUBLISHER]

The monitoring of organochlorine pesticides has raised a great concern in the last years due to their toxicity (some of them are carcinogenic and endocrine disruptor compounds) and persistence. European Directive 2008/105/EC establishes very restrictive levels for organochlorine pesticides in surface waters. Therefore, simple, fast, highly sensitive and low cost analytical methods are required to detect and quantify these pollutants in water. In the present work, four procedures for extraction and determination are proposed and compared for the analysis of 28 organochlorine pesticides in tap, surface and sea waters. The suitability of each method of analysis was evaluated for each kind of water. The extraction methods proposed were: two solid-phase extraction methods using C18laminar disk and Oasis HLB cartridges, a solid-phase microextraction procedure using a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre, and a micro liquid–liquid extraction procedure using ethyl acetate as solvent. Determination of pesticides was performed by large volume on-column injector-gas chromatography-electron capture detection (LVOCI-GC-ECD), splitless-GC-ECD and GC-MS (mass spectrometry). All methods present a good sensitivity with method detection limits lower than 10 ng L−1, good accuracy with recoveries between 75 and 120% (with some exceptions) and good precision (relative standard deviations <15%), according to the Commission Decision 2002/657/EC criteria. The advantages and disadvantages of each method are discussed in terms of the green chemistry principles, the figures of merit and the matrix effect. This work tries to be a useful guidance for routine and control analysis laboratories. [ABSTRACT FROM AUTHOR]

A method to determine 21 organochlorine pesticides in horticultural samples (lettuce, pepper, tomato, spinach and potato) based on microwave assisted extraction (MAE) followed by solid-phase extraction (SPE) clean-up is described. After extraction with hexane?:?acetone (50?:?50), a carbon cartridge was employed for the clean-up step. Pesticides were eluted with 5?mL of hexane?:?ethyl acetate (80?:?20) and determined by gas chromatography and electron capture detection (GC-ECD). Results were confirmed by GC-MS analysis. Analytical recoveries obtained were ca. 100% for most of the studied pesticides with the proposed method in each analysed matrix. The method was applied to analyse 35 commercial samples from A Coruña (NW Spain); only two samples contained pesticide residues, but none of them exceeded the MRLs established by EU legislation. [ABSTRACT FROM AUTHOR]