Abstract
BackgroundA sensitive, accurate and precise method was developed and validated in regard to Council Directive 333/2007/EC, Commission Decision 657/2002/EC, ISO/IEC 17025:2005 and EURACHEM 1998 for the trace level determination of Lead (Pb), Cadmium (Cd) and Chromium (Cr) in fish feed samples using Graphite Furnace Atomic Absorption Spectrometry (GF-AAS).MethodsFor method validation, selectivity, working and linear ranges, limit of detection (LoD), limit of quantification (LoQ), trueness (recovery) and precision (repeatability and reproducibility) have been assessed as performance criteria.ResultsThe method LoDs for Pb, Cd and Cr were found to be 0.078, 0.010 and 0.022 μg/g respectively, whereas, the method LoQs were obtained at 0.156, 0.021 and 0.044 μg/g respectively. Moreover, the recovery of the analytes was 90 – 104% and the RSD values for precision were 4.90 – 9.60% respectively.ConclusionsThe method validation performance criteria indicate the method’s suitability for trace level quantification of Pb, Cd, and Cr in fish feed samples.
Highlights
A sensitive, accurate and precise method was developed and validated in regard to Council Directive 333/2007/EC, Commission Decision 657/2002/EC, ISO/IEC 17025:2005 and EURACHEM 1998 for the trace level determination of Lead (Pb), Cadmium (Cd) and Chromium (Cr) in fish feed samples using Graphite Furnace Atomic Absorption Spectrometry (GF-AAS)
Hollow cathode lamps were used for Pb (283.3 nm and slit 0.5 nm), Cd (228.8 nm and slit 0.5 nm), and Cr (357.9 nm and slit 0.2 nm) and operated according to the conditions recommended by the manufacturer
Method validation The validation of the analytical procedure for quantitative determination of Pb, Cd, and Cr in fish feed was performed by evaluating linearity and selectivity, limit of detection (LoD), limit of quantification (LoQ), accuracy, and precision (European Commission 2007; ISO/IEC 17025 2005; EURACHEM 1998)
Summary
A sensitive, accurate and precise method was developed and validated in regard to Council Directive 333/2007/EC, Commission Decision 657/2002/EC, ISO/IEC 17025:2005 and EURACHEM 1998 for the trace level determination of Lead (Pb), Cadmium (Cd) and Chromium (Cr) in fish feed samples using Graphite Furnace Atomic Absorption Spectrometry (GF-AAS). There are several techniques available for the quantification of heavy metals at very low level, but it is essential to ensure the quality of analytical results generated by the laboratories approved for official control. For this reason, there is a growing global interest to develop and establish. Ullah et al Journal of Analytical Science and Technology (2017) 8:15 analytical methods which can provide accurate and precise measurements with low detection limit This should be achieved by practicing proper quality assurance systems and by applying methods validated following the international guidelines and standards (European Commission 2002a, 2002b, 2006, 2007, 2008). It covers testing performed using standard methods, non-standard methods, and laboratorydeveloped methods
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