Silva Larissa Pinto, Campos Náira Da Silva, Lisboa Thalles Pedrosa, de Faria Lucas Vinícius, Matos Maria Auxiliadora Costa, Matos Renato Camargo, de Sousa Rafael Arromba
BACCAN (Grupo BACCAN De Química Analítica), Departamento De Química, Instituto De Ciências Exatas, Universidade Federal De Juiz De Fora, Juiz de for A, MG, Brazil.
Instituto De Ciências Exatas, Universidade Federal De Juiz De Fora, Juiz de for A, MG, Brazil.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2021 Mar;38(3):418-426. doi: 10.1080/19440049.2020.1857443. Epub 2021 Jan 25.
In this work, an effective and simple method is proposed for the simultaneous determination of cadmium, lead and copper in chocolate samples by Square Wave Anodic Stripping Voltammetry (SWASV). An ultrasonic bath was used for the extraction of cadmium, lead and copper from fourteen chocolate samples using HNO solution (7 mol L). The electrochemical system consisted of a cell with three electrodes and HCl solution (10 mmol L) as the supporting electrolyte. An efficient extraction of the metals (~100%) was attained after 1 h of ultrasonic pre-treatment. Quantitative analysis was carried out by the standard addition method. Good linearity, precision and accuracy were obtained in the range of concentrations examined. The accuracy was evaluated by means of a reference sample of spiked skim milk powder (BCR 151) to prove the reliability of the method. Detection limits (LOD) of 0.089, 0.059 and 0.018 µg g were found for cadmium, copper and lead, respectively, in the chocolate samples. Concentrations in chocolate samples were 4.30-138 µg g for Cu and 0.83-27.9 µg g for Pb, with no significant Cd. The simultaneous determination brings advantages to other methods already reported for chocolate analysis and the samples preparation proposed avoids the traditional sample mineralization step. These characteristics show this new method is especially attractive for case studies and routine analysis.
在本研究中,提出了一种有效且简便的方法,用于通过方波阳极溶出伏安法(SWASV)同时测定巧克力样品中的镉、铅和铜。使用超声浴,以HNO₃溶液(7 mol/L)从14个巧克力样品中萃取镉、铅和铜。电化学系统由一个带有三电极的电解池和HCl溶液(10 mmol/L)作为支持电解质组成。经过1小时的超声预处理后,实现了金属的高效萃取(约100%)。采用标准加入法进行定量分析。在所检测的浓度范围内获得了良好的线性、精密度和准确度。通过添加了标准物质的脱脂奶粉参考样品(BCR 151)评估准确度,以证明该方法的可靠性。在巧克力样品中,镉、铜和铅的检测限(LOD)分别为0.089、0.059和0.018 μg/g。巧克力样品中铜的浓度为4.30 - 138 μg/g,铅的浓度为0.83 - 27.9 μg/g,未检测到显著的镉。与已报道的用于巧克力分析的其他方法相比,同时测定具有优势,并且所提出的样品制备方法避免了传统的样品矿化步骤。这些特性表明这种新方法对于案例研究和常规分析特别有吸引力。