Methylmercury determination in sediments and fish tissues from the Nerbioi-Ibaizabal estuary (Basque Country, Spain) Original Research Article

The analysis of methylmercury in extracts from environmental solid samples by gas chromatography coupled to microwave induced plasma atomic emission spectrometry (GC–MIP/AES) after the ethylation of the extract and the preconcentration of the volatile products in hexane has been critically investigated. In order to correct potential sources of random error along the analytical procedure affecting the overall repeatability of the analysis, the use of the inorganic mercury naturally occurring in the sample as internal standard in the analysis of methylmercury is proposed. A study to establish the best conditions to achieve a quantitative recovery of methylmercury without damaging its chemical structure has also been carried out. Magnetic stirring (without heating) of the sediment or fish tissue with 2 mol dm−3 HNO3 or 10% methanolic KOH, respectively, during 90 min has been considered as the most effective procedure to release methylmercury preserving its structure. The proposed method has been validated using certified reference materials (CRM-580, CRM-463 and DOLT-2), assessing its quality in terms of accuracy, repeatability and detection limit. Finally, several sediment and fish samples collected in the estuary of the Nerbioi-Ibaizabal (Bilbao, Basque Country) have been analyzed following the procedures proposed. The results obtained show the validity of the proposed method to analyze real samples.