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A rapid on-site analysis method for the simultaneous extraction and determination of Pb2+ and Cd2+ in cereals

机译:同时提取和测定谷物中Pb2 +和Cd2 +的快速现场分析方法

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In order to achieve rapid on-site screening and solve the problem of rapid pretreatment for the determination of lead (Pb ~(2+) ) and cadmium (Cd ~(2+) ) in cereals by a portable electrochemical analyzer with disposable screen-printed electrodes (SPEs), a new reliable and simple extraction method for Pb ~(2+) and Cd ~(2+) in cereals was developed. The Pb ~(2+) and Cd ~(2+) in cereals were purified by a mixed solution of 1 mol L ~(?1) potassium iodide (KI)/5% vitamin C (VC)/ethyl acetate after being extracted by 10% HNO _(3) , which transfers the Pb ~(2+) and Cd ~(2+) into ethyl acetate after a reaction with KI–VC. Then, the Pb ~(2+) and Cd ~(2+) were eluted from ethyl acetate with 5% HNO _(3) and were determined by an electrochemical analyzer with screen printed electrodes. Under the optimized conditions, the matrix calibration curves of Pb ~(2+) and Cd ~(2+) in rice and wheat showed good linear relationships with R ~(2) > 0.996. The method shows a detection limit (LOD) for Cd ~(2+) in rice and wheat of 6.7 μg kg ~(?1) and 11.5 μg kg ~(?1) , and the corresponding values for Pb ~(2+) were 34.9 and 31.1 μg kg ~(?1) , respectively. The relative standard deviation (RSD) was less than 8.7% for Cd ~(2+) and Pb ~(2+) . In addition, the recoveries of the tested reference materials using this method were between 80% and 120%. From sample pretreatment to testing results, the whole process took no more than 25 min, and the operation was simple for operators, green to the environment, cheap in terms of instruments, and above all suitable for on-site detection. The results implied that this portable electrochemical method with new pretreatment may be a good choice for screening Pb ~(2+) and Cd ~(2+) in cereal samples on-site.
机译:为了实现快速现场筛选并解决使用便携式电化学分析仪和一次性筛分仪测定谷物中铅(Pb〜(2+))和镉(Cd〜(2+)镉)的快速预处理问题,印刷电极(SPEs),开发了一种谷物中Pb〜(2+)和Cd〜(2+)的可靠,简便的提取新方法。提取后,谷物中的Pb〜(2+)和Cd〜(2+)通过1 mol L〜(?1)碘化钾(KI)/ 5%维生素C(VC)/乙酸乙酯的混合溶液进行纯化。通过10%HNO _(3),与KI–VC反应后,将Pb〜(2+)和Cd〜(2+)转移到乙酸乙酯中。然后,用5%HNO_(3)从乙酸乙酯中洗脱出Pb〜(2+)和Cd〜(2+),并通过带有丝网印刷电极的电化学分析仪进行测定。在优化条件下,水稻和小麦中Pb〜(2+)和Cd〜(2+)的基质校准曲线与R〜(2)> 0.996呈现良好的线性关系。该方法显示了水稻和小麦中Cd〜(2+)的检出限(LOD)分别为6.7μgkg〜(?1)和11.5μgkg〜(?1),以及Pb〜(2+)的相应值分别为34.9和31.1μgkg〜(?1)。 Cd〜(2+)和Pb〜(2+)的相对标准偏差(RSD)小于8.7%。此外,使用此方法测试的参考物质的回收率在80%至120%之间。从样品预处理到测试结果,整个过程只用了不到25分钟的时间,并且操作员操作简单,绿色环保,仪器价格便宜,而且最适合现场检测。结果表明,这种采用新型预处理方法的便携式电化学方法可能是现场筛选谷物样品中Pb〜(2+)和Cd〜(2+)的好选择。

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