Centro de Ciências Químicas, Farmacêuticas e de Alimentos, Universidade Federal de Pelotas, Capão do Leão, RS, 96160-000, Brazil.
Departamento de Química, Universidade Federal de Santa Maria, Santa Maria, RS, 97105-900, Brazil.
Anal Bioanal Chem. 2020 Sep;412(24):6475-6484. doi: 10.1007/s00216-020-02636-2. Epub 2020 May 12.
The halogen determination is important in view of their biological and environmental roles, but their determination has still been considered a challenge, especially at low concentrations. Therefore, a method for honey decomposition using microwave-induced combustion (MIC) combined with ion chromatography and conductimetric detection (for Cl, F, and S determination) or mass detection (for Br and I determination) (IC-CD-MS) is proposed. Trueness was evaluated by adding reference materials (RMs) or a standard solution in the sample. By using 50 mmol L NHOH as the absorbing solution, recoveries for all analytes were between 94 and 103%, in both tests. Moreover, no statistical difference (t test, confidence level of 95%) was observed for the results obtained by IC in comparison with those obtained by inductively coupled plasma optical emission spectroscopy (Cl and S) and by inductively coupled plasma mass spectrometry (Br and I). Finally, the proposed method was applied to 19 honey samples from different origins. The concentrations ranged from < 0.45 to 2.39 mg kg (Br), 21.8 to 671 mg kg (Cl), and 11 to 154 mg kg (S), while the F and I concentrations were below that their quantification limits (LOQs) in all analyzed samples. The LOQs for Br, Cl, F, I, and S were 0.45, 21, 3.7, 0.077, and 8.7 mg kg, respectively. The MIC method provided a compatible solution to IC for the halogen and S determination in honey by a single analysis. Graphical abstract.
鉴于卤素的生物和环境作用，其测定很重要，但由于其浓度较低，测定一直被认为是一个挑战。因此，提出了一种使用微波诱导燃烧（MIC）结合离子色谱和电导检测（用于测定 Cl、F 和 S）或质量检测（用于测定 Br 和 I）（IC-CD-MS）对蜂蜜进行分解的方法。通过在样品中添加参考物质（RMs）或标准溶液来评估准确性。使用 50 mmol L NHOH 作为吸收溶液，所有分析物的回收率在两种测试中均在 94%至 103%之间。此外，通过 IC 获得的结果与通过电感耦合等离子体发射光谱法（Cl 和 S）和电感耦合等离子体质谱法（Br 和 I）获得的结果之间没有统计学差异（t 检验，置信水平为 95%）。最后，将所提出的方法应用于来自不同来源的 19 个蜂蜜样品。浓度范围为 <0.45 至 2.39 mg kg（Br），21.8 至 671 mg kg（Cl）和 11 至 154 mg kg（S），而所有分析样品中的 F 和 I 浓度均低于其定量限（LOQs）。Br、Cl、F、I 和 S 的 LOQs 分别为 0.45、21、3.7、0.077 和 8.7 mg kg。MIC 方法为 IC 提供了一种兼容的解决方案，可通过单次分析测定蜂蜜中的卤素和 S。
