López-García Ignacio, Viñas Pilar, Romero-Romero Rafael, Hernández-Córdoba Manuel
Department of Analytical Chemistry, University of Murcia, Murcia E-30071, Spain.
Talanta. 2009 Jun 15;78(4-5):1458-63. doi: 10.1016/j.talanta.2009.02.045. Epub 2009 Mar 5.
A new method for the electrothermal atomic absorption spectrometric determination of vanadium in milk and infant formulas using suspensions to avoid the need for previous dissolution of samples is described. Sensitivity is improved by a procedure based on preconcentration and removal of the matrix, using ion-exchange (Dowex 1X8-100). Suspensions of 15% (m/v) infant formula samples were prepared in a medium containing 0.05M sodium citrate (pH 7.2) and passed through the ion exchange column. Vanadium was eluted from the column using 1M hydrochloric acid and injected in the graphite furnace using a mixture of hydrofluoric acid plus magnesium nitrate as chemical modifiers. Calibration was carried out using multiple injection and aqueous standards prepared in the same medium. Detection limits were 0.2 ng g(-1) for infant formulas and 0.02 microg L(-1) for cow milk samples. The reliability of the procedure was checked by comparing the results obtained with those found using a previous mineralization stage and by analyzing five certified reference materials.
本文描述了一种电热原子吸收光谱法测定牛奶和婴儿配方奶粉中钒的新方法,该方法使用悬浮液,无需预先溶解样品。通过基于离子交换(Dowex 1X8 - 100)的预浓缩和去除基质的程序提高了灵敏度。在含有0.05M柠檬酸钠(pH 7.2)的介质中制备15%(m/v)婴儿配方奶粉样品的悬浮液,并使其通过离子交换柱。使用1M盐酸从柱上洗脱钒,并使用氢氟酸加硝酸镁的混合物作为化学改进剂将其注入石墨炉中。使用多次进样和在相同介质中制备的水溶液标准品进行校准。婴儿配方奶粉的检测限为0.2 ng g(-1),牛奶样品的检测限为0.02 μg L(-1)。通过将所得结果与使用先前矿化阶段获得的结果进行比较,并分析五种有证标准物质,检验了该程序的可靠性。