Validation of lead determination in fish and shellfish, by a graphite furnace atomic absorption spectrometry (GFAAS) method

Validation is the process of demonstrating or confirming the performance characteristics of a method of analysis.In our study, we used the standard Moroccan NM 08.0.056 2007 to validate the method for determining lead in fish.A graphite furnace atomic absorption spectrophotometry(GFAAS)method, based on AOAC 999.10 (AOAC 2002) , and optimized and validated in our laboratory was used to determine lead at specific levels in routine analysis of fish.The validation was carried out according to four levels of experience (A, B, C and D), the design of experiments type "A" to characterize the linearity, limits of detection (LD) and quantification (LQ) of calibration curve, the plan "B" for the control of matrix effects (specificity) of the method, the plan "C" for estimating the precision (repeatability internal), the accuracy and repeatability possible internal; and plan "D" (optional) that will be used to calculate the internal reproducibility. The lead data was assessed for compliance with the methods performance criteria guidelines laid down in NM 08.0.056. calibration was carried out and linearity was obtained in the working ranges: 3-30 μg/l, specificity and accuracy at the intervals tested in good agreement with the requirements, although our detection and quantification limit were above the established limits in the directive (LD = 0.0015 ppb, LQ = 0.005 ppb)