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A rapid on-site analysis method for the simultaneous extraction and determination of Pb2+ and Cd2+ in cereals
Authors:Ming-hui Zhou  Wei Tian  Jie-qiong Zhang  Xi Chen  Yan-xiang Wu  Song-xue Wang
Institution:The Academy of National Food and Strategic Reserves Administration (Former Name: Academy of State Administration of Grain, ab. ASAG), No. 11 Baiwanzhuang Str., Xicheng District, Beijing 100037 China,
Abstract:In order to achieve rapid on-site screening and solve the problem of rapid pretreatment for the determination of lead (Pb2+) and cadmium (Cd2+) in cereals by a portable electrochemical analyzer with disposable screen-printed electrodes (SPEs), a new reliable and simple extraction method for Pb2+ and Cd2+ in cereals was developed. The Pb2+ and Cd2+ 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% HNO3, which transfers the Pb2+ and Cd2+ into ethyl acetate after a reaction with KI–VC. Then, the Pb2+ and Cd2+ were eluted from ethyl acetate with 5% HNO3 and were determined by an electrochemical analyzer with screen printed electrodes. Under the optimized conditions, the matrix calibration curves of Pb2+ and Cd2+ in rice and wheat showed good linear relationships with R2 > 0.996. The method shows a detection limit (LOD) for Cd2+ in rice and wheat of 6.7 μg kg−1 and 11.5 μg kg−1, and the corresponding values for Pb2+ were 34.9 and 31.1 μg kg−1, respectively. The relative standard deviation (RSD) was less than 8.7% for Cd2+ and Pb2+. 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 Pb2+ and Cd2+ in cereal samples on-site.

To achieve rapid on-site screening rapid pretreatment for the determination of Pb2+ and Cd2+ in cereals by a portable electrochemical analyzer with disposable screen-printed electrodes, a new reliable and simple extraction method for Pb2+ and Cd2+ was developed.
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