Wang Shuo, Dong Xv, Dai Bingye, Pan Mingfei, He Shaoyuan, Wang Junping
Tianjin University of Science & Technology, Ministry of Education of China, Key Laboratory of Food Nutrition and Safety, Tianjin 300457, People's Republic of China.
J AOAC Int. 2015 Jan-Feb;98(1):218-24. doi: 10.5740/jaoacint.11-476.
A method was developed for detection of V, Cr, Cu, As, and Pb in water and biological samples by combining online flow injection and preconcentration with inductively coupled plasma-MS. The 2-nitroso-1-naphthol-4-sulfonic acid (Nitroso-S) impregnated MCI GEL CHP20P resin was prepared as an enrichment sorbent. Some parameters affecting the efficiency of the preconcentration process were investigated in the experiment, including the pH and volume of sample solution, the flow rate for sample loading, the type and concentration of eluent, and the influence of co-existing ions. Under the optimal experimental conditions, the enrichment factor and LOD (3s) of chosen metal ions V, Cr, Cu, As, and Pb were in the ranges of 71-268 and 4.89-23.76 ng/L, respectively. Based on 11 repeated measurements of standard solutions (1.0 μg/L), the RSD of the ions ranged from 1.2 to 2.9%. The detection procedure was also performed for analyzing two certified reference materials, GBW 08607 (water) and GBW 10052 (green tea), as well as environmental water and biological samples. Good agreement with certified values and high recoveries have demonstrated improved accuracy of the proposed method.
建立了一种将在线流动注射和预富集与电感耦合等离子体质谱相结合的方法，用于检测水和生物样品中的钒、铬、铜、砷和铅。制备了负载2-亚硝基-1-萘酚-4-磺酸（亚硝基-S）的MCI GEL CHP20P树脂作为富集吸附剂。实验中研究了一些影响预富集过程效率的参数，包括样品溶液的pH值和体积、进样流速、洗脱剂的类型和浓度以及共存离子的影响。在最佳实验条件下，所选金属离子钒、铬、铜、砷和铅的富集因子和检出限（3s）分别在71-268和4.89-23.76 ng/L范围内。基于对1.0 μg/L标准溶液进行11次重复测量，离子的相对标准偏差在1.2%至2.9%之间。还对两种有证标准物质GBW 08607（水）和GBW 10052（绿茶）以及环境水样和生物样品进行了检测。与认定值的良好一致性和高回收率证明了该方法的准确性有所提高。
