Development and Validation of a Spectrometric Method for Cd and Pb Determination in Zeolites and Safety Evaluation

Abstract

An analytical method based on microwave-assisted acid digestion and atomic absorption spectrometry with graphite furnace as atomization source was developed and validated for determining trace elements (Cd and Pb) in zeolites used as dietary supplements, for their characterization and safety evaluation. The method was checked for the main performance parameters according to the legislation requirements in the field of dietary supplements. In all cases, the obtained performance parameters were satisfactory. The selectivity study showed no significant non-spectral matrix effect. The linearity study was conducted for the calibration curves in the range of 0–10 ng mL−1 for Cd and 0–30 ng mL−1 for Pb. The obtained limits of detection (LoDs) and the limits of quantification (LoQs) were sufficiently low in order to allow Pb and Cd determination in dietary supplements. For the internal quality control, certified reference materials were analysed and good recoveries were obtained. The precision study was performed in terms of repeatability and reproducibility, considering the requirements imposed by the Commission Decision (2007/333/EC) and the method fulfilled these performance parameters. Expanded measurement uncertainties were estimated to 11% for Cd and 10% for Pb. Cd and Pb content were measured in real zeolite samples and, using these data, a safety evaluation was carried out.