Department of Chemistry, Federal University of Minas Gerais, PO Box 702, 31270-901 Belo Horizonte, Minas Gerais, Brazil; Federal Institute of Education, Science and Technology of North of Minas Gerais, IFNMG Campus Almenara, Brazil.
Department of Chemistry, Federal University of Minas Gerais, PO Box 702, 31270-901 Belo Horizonte, Minas Gerais, Brazil.
Talanta. 2017 Nov 1;174:274-278. doi: 10.1016/j.talanta.2017.05.059. Epub 2017 May 22.
A method of direct analysis for quantification of 15 inorganic elements (P, S, Cl, K, Ca, Mn, Fe, Ni, Cu, Zn, Br, As, Rb, Sr and Pb) in beers by Total Reflection X-Ray Fluorescence (TXRF) was developed. The experimental conditions were optimized. Direct analysis was compared with the acid digestion procedure to evaluate the effect matrix and the results were satisfactory. The evaluation of the accuracy and precision was realized by analysis of two certified reference materials of natural and waste water. For the majority of the elements, good agreement was achieved between the certified value and the value measured in the CRM´s. Low detection limits were obtained and it was adequate to determine trace elements in beers and to quality control Pb and As, whose maximum limits are 200 and 100µgL, respectively. The relative standard deviation (RSD%) ranged from 2.4% to 10%. The method was applied to 30 beer samples collected in several regions of Brazil. The concentration ranges (mgL) for the studied analytes were: P: (37.40-140.85); S (10.32-50.73); Cl (82.74-281.7); K (183.8-418.5); Ca (9.82-96.0); Mn (0.06-1.42); Fe (0.07-1.57); Ni (< LLD-1.13); Cu (< LLD-0.32); Zn (0.02-1.98); As (< LLD-0.10); Br (0.01-2.04); Rb (< LLD-0.52); Sr (< LLD-0.41) and Pb (< LLD-0.18). Some beer samples showed As and Pb concentrations above the levels established by Brazilian legislation. The developed method is simple, fast, consumes low amounts of reagents and allows the determination of a large number of analytes simultaneously. TXRF proved to be attractive and useful for routine analysis.
建立了一种通过全反射 X 射线荧光(TXRF)直接分析啤酒中 15 种无机元素(P、S、Cl、K、Ca、Mn、Fe、Ni、Cu、Zn、Br、As、Rb、Sr 和 Pb)的定量分析方法。优化了实验条件。直接分析与酸消解程序进行了比较,以评估基质的影响,结果令人满意。通过分析两种天然和废水的认证参考材料来实现对准确性和精密度的评估。对于大多数元素,在 CRM 中测量的结果与认证值之间都达成了良好的一致性。获得了低检测限,足以用于测定啤酒中的微量元素,并用于质量控制 Pb 和 As,其最大限量分别为 200 和 100μg/L。相对标准偏差(RSD%)范围为 2.4%至 10%。该方法应用于在巴西多个地区采集的 30 个啤酒样品。所研究分析物的浓度范围(mg/L)为:P:(37.40-140.85);S(10.32-50.73);Cl(82.74-281.7);K(183.8-418.5);Ca(9.82-96.0);Mn(0.06-1.42);Fe(0.07-1.57);Ni(< LLD-1.13);Cu(< LLD-0.32);Zn(0.02-1.98);As(< LLD-0.10);Br(0.01-2.04);Rb(< LLD-0.52);Sr(< LLD-0.41)和 Pb(< LLD-0.18)。一些啤酒样品的 As 和 Pb 浓度超过了巴西法规规定的水平。所开发的方法简单、快速,试剂消耗量低,允许同时测定大量分析物。TXRF 被证明是一种有吸引力且有用的常规分析方法。