Lo Coco F, Monotti P, Novelli V, Ceccon L, Adami G, Micali G
Department of Economic Sciences, University of Udine, Via Tomadini 30/A, I-33100, Italy.
Food Addit Contam. 2004 May;21(5):441-6. doi: 10.1080/02652030410001677754.
A method for the determination of cadmium and lead in vegetables by stripping chronopotentiometric analysis, after digestion of the sample with concentrated sulphuric acid and dry-ashing, is described. Metal ions were concentrated as their amalgams on a glassy carbon-working electrode previously coated with a thin mercury film and then stripped by a suitable oxidant. Potential and time data were digitally derived and E was plotted versus dt/dE(-1), thus increasing both the sensitivity of the method and the resolution of the analysis. Quantitative analysis was carried out by the method of standard addition; good linearity was obtained in the range of examined concentrations, as was shown by the determination coefficients, which were 0.998 (n = 4) for cadmium and 0.993 (n = 4) for lead. Recoveries of 85-100% for cadmium and of 84-97% for lead were obtained from a sample spiked at different levels. Accuracy was demonstrated by analysis of a matching reference sample of cabbage. The detection limits were 1.8 ng g(-1) of wet mass for cadmium and 5.1 ng g(-1) of wet mass for lead. The relative standard deviations (mean of nine determinations), evaluated on a real sample, were 6.7 and 6.2%, respectively. Results obtained on 10 different commercial samples of pepper (Capsicum annuum), and egg plant (Solanum melongena) were not significantly different from those obtained by graphite furnace atomic absorption spectrophotometry technique. The average content was in the range 3.1-18.6 ng g(-1) for cadmium and 38.2-64.3 ng g(-1) for lead.
本文描述了一种通过溶出计时电位分析法测定蔬菜中镉和铅的方法。样品经浓硫酸消解和干灰化处理后进行分析。金属离子以汞齐形式富集在预先涂有薄汞膜的玻碳工作电极上,然后用合适的氧化剂进行溶出。通过数字方式获取电位和时间数据,并绘制E与dt/dE(-1)的关系图,从而提高了该方法的灵敏度和分析分辨率。采用标准加入法进行定量分析;在所研究的浓度范围内获得了良好的线性关系,镉的测定系数为0.998(n = 4),铅的测定系数为0.993(n = 4)。在不同加标水平的样品中,镉的回收率为85 - 100%,铅的回收率为84 - 97%。通过分析匹配的卷心菜参考样品证明了该方法的准确性。镉的检测限为湿质量1.8 ng g(-1),铅的检测限为湿质量5.1 ng g(-1)。对实际样品进行九次测定的相对标准偏差分别为6.7%和6.2%。在10种不同的市售辣椒(辣椒属)和茄子(茄属)样品上获得的结果与石墨炉原子吸收光谱法所得结果无显著差异。镉的平均含量范围为3.1 - 18.6 ng g(-1),铅的平均含量范围为38.2 - 64.3 ng g(-1)。