Development, validation, and accreditation of a method for the determination of 75As, 111Cd, 201Hg, and 208Pb in Cephalopods using inductively coupled plasma mass spectrometry (ICP-MS)

Abstract

A sensitive, accurate and precise method was developed and validated for the trace level determination of 75As, 111Cd, 201Hg, and 208Pb in Cephalopods using inductively coupled plasma mass spectrometry. The selectivity and linearity, limit of detection (LOD) and limit of quantification (LOQ), recovery study, repeatability and within-laboratory reproducibility, Horwitz ratio (HORRAT), measurement uncertainty and fitness of purpose of the method were determined. The LOD for 75As, 111Cd, 201Hg, and 208Pb were found to be 14.68, 12.70, 5.13, and 2.74 µg/kg respectively whereas, the LOQ obtained were 48.94, 42.33, 17.11 and 9.13 µg/kg respectively. The relative standard deviation for the repeatability and within-laboratory reproducibility for all determined trace elements were below 3 and 16%, respectively. The HORRATr and HORRATR values of repeatability and reproducibility were lower than 2. Furthermore, the recovery values of the spiked samples ranged from 81.79 to 101.67%. These results complied with the performance criteria established by Council Regulation (EC) 333/2007 and the clause 5.4.5.2, ISO/IEC 17025:2005. Therefore, the procedure is implemented for the routine analysis to determine trace level quantification of 75As, 111Cd, 201Hg, and 208Pb in Cephalopods.