Centro de Ciências Químicas, Farmacêuticas e de Alimentos, Universidade Federal de Pelotas, 96160-000, Capão do Leão, RS, Brazil.
Departamento de Química, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS, Brazil.
Anal Chim Acta. 2019 Jul 4;1060:45-52. doi: 10.1016/j.aca.2019.01.032. Epub 2019 Jan 25.
An effective analytical method for bromine and iodine determination in human hair using interference-free inductively coupled plasma mass spectrometry (ICP-MS) was developed. Human hair was digested based on combustion reaction to obtain compatible solutions with ICP-MS analysis. Using microwave-induced combustion (MIC), masses of human hair ranging from 50 to 300 mg were efficiently digested. Only a diluted alkaline solution (100 mmol L NHOH) was used for the absorption of both analytes, which was fully compatible with ICP-MS analysis. Using these conditions low limits of detection were obtained (LOD of 0.01 μg g for Br and 0.004 μg g for I). Recovery tests at two levels (50% and 100%) using a standard solution or mixtures of the sample with certified reference materials (CRMs) were carried out to evaluate the suitability of proposed method and recoveries between 94% and 102% were always obtained. Accuracy was evaluated by analysis of a human hair CRM, and the Br and I concentrations obtained by the proposed method did not differ significantly from those described in the certificate. Repeatability (RSDs ≤ 4%) and reproducibility (RSDs ≤ 7%) of the results using proposed method were always very suitable. The digests obtained using the MIC method were fully compatible with ICP-MS and the interferences currently found using conventional digestion methods were completely eliminated. Ultra-trace concentrations of Br and I were determined in human hair, demonstrating that the proposed method is a suitable strategy, and it presents several advantages compared to others published in the literature.
开发了一种使用无干扰电感耦合等离子体质谱法(ICP-MS)测定人发中溴和碘的有效分析方法。基于燃烧反应,将人发消解,得到与 ICP-MS 分析相容的溶液。使用微波诱导燃烧(MIC),可有效消解 50-300mg 质量的人发。仅使用稀释的碱性溶液(100mmolLNHOH)吸收两种分析物,完全与 ICP-MS 分析兼容。使用这些条件,获得了较低的检测限(Br 的检测限为 0.01μg/g,I 的检测限为 0.004μg/g)。使用标准溶液或样品与认证参考物质(CRM)的混合物进行两个水平(50%和 100%)的回收测试,以评估所提出方法的适用性,回收率始终在 94%至 102%之间。通过分析人发 CRM 来评估准确性,所提出方法获得的 Br 和 I 浓度与证书中描述的浓度没有显著差异。使用所提出方法的结果的重复性(RSDs≤4%)和再现性(RSDs≤7%)始终非常适合。使用 MIC 方法获得的消解物与 ICP-MS 完全兼容,并且完全消除了目前在常规消解方法中发现的干扰。在人发中测定了痕量的 Br 和 I,证明该方法是一种合适的策略,与文献中公布的其他方法相比具有几个优势。