Centro de Ciências Químicas, Farmacêuticas e de Alimentos, Universidade Federal de Pelotas, Capão do Leão, RS, Brazil.
Departamento de Química, Universidade Federal de Santa Maria, Santa Maria, RS, Brazil.
Rapid Commun Mass Spectrom. 2020 Sep;34 Suppl 3:e8675. doi: 10.1002/rcm.8675. Epub 2020 Feb 25.
Bromine and iodine have important physiological functions; however, in inadequate concentration, they can also cause several physiological problems. Their mobility assessment in human organisms through biological sampling may help clarify some doubts related to metabolic routes, which are still not well elucidated. In this context, a suitable analytical method for this purpose should be developed.
An analytical method for determining ultratrace levels of bromine and iodine in human nail samples was developed. Inductively coupled plasma mass spectrometry (ICP-MS) using a conventional nebulization system was immediately chosen as the determination tool because of its powerful sensitivity and selectivity. Sample preparation methods including microwave-induced combustion (MIC), microwave-assisted extraction, and microwave-assisted digestion were evaluated. The compatibility of the final solutions with ICP-MS analysis was considered while the method was developed.
MIC was chosen as the most suitable method for the sample preparation for determining the levels of bromine and iodine in human nail samples using ICP-MS. Unlike other sample preparation methods, this one fully eliminated interferences related to the carbon content and memory effects. Sample masses up to 100 mg were efficiently digested, and the analytes were quantitatively absorbed using only 50 mmol L NH OH solution. Recoveries ranged from 93% to 102%, and the relative standard deviation was < 8%.
The proposed analytical method presents important characteristics for routine analysis. It allows ultratrace determination even when low sample masses are used because of the low blank values, reduced volume of reagents, and powerful detectability using ICP-MS.
溴和碘具有重要的生理功能;然而,在浓度不足的情况下,它们也会引起一些生理问题。通过生物样本对人体中这些元素的移动性进行评估,可能有助于阐明一些代谢途径方面仍不清楚的问题。在这种情况下,应该开发一种合适的分析方法。
开发了一种用于测定人指甲样本中痕量溴和碘的分析方法。由于电感耦合等离子体质谱法(ICP-MS)具有强大的灵敏度和选择性,因此立即选择了常规雾化系统的 ICP-MS 作为测定工具。评估了包括微波诱导燃烧(MIC)、微波辅助提取和微波辅助消解在内的几种样品制备方法。在开发方法的同时,还考虑了最终溶液与 ICP-MS 分析的兼容性。
MIC 被选为使用 ICP-MS 测定人指甲样本中溴和碘水平的最适合的样品制备方法。与其他样品制备方法不同,该方法完全消除了与碳含量有关的干扰和记忆效应。可以有效地消解高达 100mg 的样品量,只需使用 50mmol/L NH OH 溶液即可定量吸收分析物。回收率在 93%至 102%之间,相对标准偏差小于 8%。
所提出的分析方法具有重要的常规分析特点。由于空白值低、试剂用量少以及 ICP-MS 的高检测能力,即使使用低质量的样本也可以进行痕量测定。