Jornal de Cromatografia e Técnicas de Separação
Acesso livre

Abstrato

Comprehensive Method Validation for the Determination of As, Cd, Hg and Pb in Cephalopods with its Applicability in Crustaceans and Fish Using ICPMS: The Role of Measurement Uncertainty for Reporting Statement of Conformity

Kajan Kumar, Anoop A. Krishnan*, B. Vijaykumar, Lijo John, M. Kaliraj, T. Maheswara Rao, JayapalanG, J.S. Reddy

A simple, sensitive, accurate and precise Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) method after microwave-assisted digestion was validated comprehensively for determination of arsenic, cadmium, mercury and lead in cephalopods and its applicability in crustaceans and fin fish samples. The performance characteristics like specificity, trueness, recovery, repeatability and intermediate repeatability with evaluation of HORRAT, Limit of Determination (LOD), Limit of Quantification (LOQ), standard measurement uncertainty and fitness for purpose is reported. The results of method validation demonstrated that the method complies with the performance criteria as per European Commission regulation 333/2007/EC. The ERM-CE278K (Mussel Tissue) certified reference material was used to evaluate trueness of the method. The mean recovery ranged between 82 to 120%. The HORRAT values were less than 2 for all concentration ranges studied. The method produced results with a combined standard measurement uncertainty (u) less than the maximum standard measurement uncertainty (uf), ensured its suitability for official control. The paper brought out the role of measurement uncertainty in reporting statement of conformity as per ISO/IEC 17025: 2017. The method described can be considered adequate for the simultaneous determination and quantification of the chosen toxic element in seafood and can also be applied in official control samples.