Method development for the control determination of mercury in seafood by solid-sampling thermal decomposition amalgamation atomic absorption spectrometry (TDA AAS)

Abstract

A very simple and rapid method for the determination of total mercury in fish samples using the Direct Mercury Analyser DMA-80 was developed. In this system, a previously weighted portion of fresh fish is combusted and the released mercury is selectively trapped in a gold amalgamator. Upon heating, mercury is desorbed from the amalgamator, an atomic absorption measurement is performed and the mercury concentration is calculated. Some experimental parameters have been studied and optimised. In this study the sample mass was about 100.0 mg. The relative standard deviation was lower than 8.0% for all measurements of solid samples. Two calibration curves against aqueous standard solutions were prepared through the low linear range from 2.5 to 20.0 ng of Hg, and the high linear range from 25.0 to 200.0 ng of Hg, for which a correlation coefficient better than 0.997 was achieved, as well as a normal distribution of the residuals. Mercury reference solutions were prepared in 5.0% v/v nitric acid medium. Lyophilised fish tissues were also analysed; however, the additional procedure had no advantage over the direct analysis of the fresh fish, and additionally increased the total analytical process time. A fish tissue reference material, IAEA-407, was analysed and the mercury concentration was in agreement with the certified value, according to the t-test at a 95% confidence level. The limit of quantification (LOQ), based on a mercury-free sample, was 3.0 µg kg⁻¹. This LOQ is in accordance with performance criteria required by the Commission Regulation No. 333/2007. Simplicity and high efficiency, without the need for any sample preparation procedure, are some of the qualities of the proposed method.

Keywords:

• statistical analysis
• metal determination – AAS
• method validation
• quality assurance
• environmental contaminants
• heavy metals – mercury
• trace elements (toxic)
• fish and fish products
• seafood

Acknowledgements

The authors are thankful to the Ministério da Agricultura, Pecuária e Abastecimento (MAPA) for financial support, and to the Conselho Nacional de Pesquisa e Desenvolvimento Tecnológico (CNPq, Brazil) for a scholarship (D. P. Torres). The invaluable contributions of Angelo de Queiroz Mauricio, Maria de Fátima Martins Pinhel, Carolina Costa Mota Paraiba and Roy Edward Bruns are acknowledged.