Centro de Ciências Químicas, Farmacêuticas e de Alimentos, Universidade Federal de Pelotas, Capão do Leão, RS, 96160-000, Brazil.
Anal Bioanal Chem. 2019 Jul;411(19):4873-4881. doi: 10.1007/s00216-019-01733-1. Epub 2019 May 31.
A single analysis of hair for determining halogens (chlorine, bromine, fluorine, and iodine) and sulfur by ion chromatography with suppressed conductivity and mass spectrometry detection (IC-MS) was proposed. Inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry (ICP-MS) were also used to compare the results. For this purpose, 300 mg of human hair were digested by microwave-induced combustion (MIC) using 20 bar of oxygen pressure. The analytes were absorbed in 100 mmol L NHOH. Trueness of the proposed method was evaluated by analysis of a CRM of human hair; by recovery tests, using standard solution at two levels (50% and 100%), and by comparison of results with those obtained by ICP OES (Cl and S) and ICP-MS (Br and I). Suitable recoveries (ranging from 92 to 105%) were obtained, and the results from CRM analysis did not differ significantly from those described in the certificate. Moreover, results obtained by IC-MS did not present significant differences (p > 0.05) from those obtained by ICP OES and by ICP-MS. Precision was evaluated in terms of repeatability and intermediate precision, and the relative standard deviations were always lower than 8%. The proposed method presented good accuracy and it is a reliable strategy for human hair analysis. Final digests obtained using the MIC method were fully compatible with all proposed determination techniques. Compared to others reported in the literature, the proposed method presents several advantages, especially given that it is possible to determine halogens and sulfur in a single analysis. Graphical abstract.
提出了一种通过离子色谱抑制电导和质谱检测（IC-MS）分析头发中卤素（氯、溴、氟和碘）和硫的单一分析方法。还使用电感耦合等离子体发射光谱法（ICP-OES）和电感耦合等离子体质谱法（ICP-MS）进行了比较。为此，使用 20 巴氧气压力的微波诱导燃烧（MIC）对 300mg 人发进行消解。将分析物吸收在 100mmol/L NHOH 中。通过分析人发 CRM 评估所提议方法的准确性；通过使用两个水平（50%和 100%）的标准溶液进行回收测试，并通过与 ICP-OES（Cl 和 S）和 ICP-MS（Br 和 I）获得的结果进行比较来评估准确性。获得了适当的回收率（范围为 92%至 105%），并且 CRM 分析的结果与证书中描述的结果没有显着差异。此外，IC-MS 获得的结果与 ICP-OES 和 ICP-MS 获得的结果没有显着差异（p>0.05）。以重复性和中间精密度评估精密度，相对标准偏差始终低于 8%。所提出的方法具有良好的准确性，是一种可靠的人发分析策略。使用 MIC 方法获得的最终消解物与所有提议的测定技术完全兼容。与文献中报道的其他方法相比，该方法具有许多优点，特别是可以在单次分析中同时测定卤素和硫。
