Departamento de Química, Universidade Federal de Santa Maria, Santa Maria, RS, 97105-900, Brazil.
Centro de Ciências Químicas, Farmacêuticas e de Alimentos, Universidade Federal de Pelotas, Capão do Leão, RS, 96160-000, Brazil.
Anal Bioanal Chem. 2024 May;416(11):2859-2870. doi: 10.1007/s00216-024-05235-7. Epub 2024 Mar 9.
Microwave-induced combustion (MIC) was proposed in this study for honey decomposition aiming for As, Cd, Hg, and Pb determination by inductively coupled plasma mass spectrometry (ICP-MS). Sample mass (up to 1.0 g), absorbing solution (0.5 to 14.4 mol L HNO, and HO), heating program, and combustion aids were evaluated. The Eurachem guidelines were used for method validation. The proposed method enabled combustion of a high sample mass (0.8 g of honey, with 0.4 g of microcrystalline cellulose and 100 µL of 6 mol L NHNO) using 6 mL of an absorbing solution consisting of 1 mol L HNO, which resulted in low residual carbon in solution (< 25 mg L). Honey samples from different geographical origins were analyzed. Results showed no significant difference in comparison to other two microwave decomposition methods, based on microwave-assisted wet digestion with single reaction chamber (MAWD-SRC) and microwave-assisted wet digestion (MAWD). Standard addition experiments resulted in recoveries higher than 98%. The limits of detection ranged from 1.10 (As) to 4.60 ng g (Pb). In addition to using only diluted reagents and resulting in digests virtually free of interferences, the proposed method was faster (< 30 min) than most of those presented in the literature.
本研究提出了微波诱导燃烧（MIC）方法，用于蜂蜜中砷、镉、汞和铅的电感耦合等离子体质谱（ICP-MS）测定。评估了样品质量（高达 1.0 g）、吸收液（0.5 至 14.4 mol L HNO 和 HO）、加热程序和助燃剂。方法验证遵循 Eurachem 指南。该方法可使用 6 mL 吸收液（含 1 mol L HNO）燃烧高样品质量（0.8 g 蜂蜜，含 0.4 g 微晶纤维素和 100 µL 6 mol L NHNO），从而使溶液中残留的碳量低（<25 mg L）。分析了来自不同地理来源的蜂蜜样品。与基于单反应室微波辅助湿式消解（MAWD-SRC）和微波辅助湿式消解（MAWD）的两种微波分解方法相比，结果无显著差异。标准添加实验的回收率高于 98%。检出限范围为 1.10（As）至 4.60 ng g（Pb）。与文献中大多数方法相比，该方法仅使用稀释试剂，且消解液几乎无干扰，速度更快（<30 min）。
