de Melo Malinowski Maiara Helena, Maciel Paloma Konzgen, Chaves Marisa de Jesus Silva, Barbosa Sergiane Caldas, Primel Ednei Gilberto, Duarte Fábio Andrei, Soares Bruno Meira
Escola de Química e Alimentos, Universidade Federal do Rio Grande, 96203-900, Rio Grande, RS, Brazil.
Departamento de Química, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS, Brazil.
Talanta. 2022 Jul 1;244:123395. doi: 10.1016/j.talanta.2022.123395. Epub 2022 Mar 17.
Edible seaweed has been widely consumed around the world through oriental cuisine and it is important to monitor the levels of some elements, especially halogens. This study proposes, for the first time, the development of an analytical method using the vortex-assisted matrix solid-phase dispersion (VA-MSPD) combined with alkaline extraction of halogens (F, Cl, Br, and I) in edible seaweed for further determination by ion chromatography. The proposed method was evaluated using edible seaweed of the Nori (Porphyra spp.) type and applied to samples of the Wakame (Undaria pinnatifida), Kombu (Laminaria ochroleuca), and Hijiki (Hizikia fusiformis) types. Important VA-MSPD parameters were investigated and using 0.1 g sample, 1 g sea sand as solid support, 50 mmol L (NH)CO as extraction solution, and 5 min of maceration, higher extraction efficiencies were obtained. The method was linear within the evaluated range (R > 0.99) for all elements and no matrix effect was observed. The detection limits of the method were 27, 26, 19, and 28 μg g for F, Cl, Br, and I, respectively. The accuracy was evaluated by a recovery test (ranging from 92 to 108%) and analysis of certified reference materials for apple leaves (NIST 1515) and peach leaves (NIST 1547), which had a good agreement (ranging from 97 to 101%) with the certified values. Comparing the results with those obtained by inductively coupled plasma-mass spectrometry after microwave-induced combustion, no significant difference was found between the results, and the relative standard deviations were lower than 12%. The proposed method proved to be efficient for the determination of halogens in different algae species, showing advantages such as simplicity and low cost, combined to the use of a material from renewable sources (sea sand) as a solid support, contributing to the principles of Green Analytical Chemistry.
可食用海藻通过东方美食在世界各地被广泛食用，监测某些元素的含量，尤其是卤素含量，非常重要。本研究首次提出开发一种分析方法，即采用涡旋辅助基质固相分散法（VA-MSPD）结合可食用海藻中卤素（氟、氯、溴和碘）的碱性萃取，以便通过离子色谱法进行进一步测定。使用紫菜（紫菜属）类型的可食用海藻对所提出的方法进行了评估，并将其应用于裙带菜（裙带菜）、海带（半叶马尾藻）和羊栖菜（羊栖菜）类型的样品。研究了重要的VA-MSPD参数，使用0.1 g样品、1 g海砂作为固相载体、50 mmol L（NH）CO作为萃取溶液并浸泡5分钟，获得了更高的萃取效率。该方法在评估范围内对所有元素均呈线性（R>0.99），且未观察到基质效应。该方法对氟、氯、溴和碘的检出限分别为27、26、19和28 μg g。通过回收率测试（92%至108%）以及对苹果叶（NIST 1515）和桃叶（NIST 1547）标准参考物质的分析来评估准确性，其与认证值具有良好的一致性（97%至101%）。将结果与微波诱导燃烧后电感耦合等离子体质谱法获得的结果进行比较，结果之间未发现显著差异，相对标准偏差低于12%。所提出的方法被证明对不同藻类物种中卤素的测定有效，具有简单、低成本等优点，同时使用可再生资源（海砂）作为固相载体，符合绿色分析化学的原则。
