Environmental Biotechnology Laboratory (BioTA), Faculty of Exact and Natural Sciences, National University of Cuyo, Interdisciplinary Institute of Basic Sciences (ICB), UNCUYO-CONICET, Padre J. Contreras 1300, 5500, Mendoza, Argentina.
Laboratory of Analytical Chemistry for Research and Development (QUIANID), Faculty of Exact and Natural Sciences, National University of Cuyo, Interdisciplinary Institute of Basic Sciences (ICB), UNCUYO-CONICET, Padre J. Contreras 1300, 5500, Mendoza, Argentina.
Anal Bioanal Chem. 2023 Sep;415(22):5475-5486. doi: 10.1007/s00216-023-04821-5. Epub 2023 Jul 3.
A new hybrid bionanomaterial composed of graphene oxide (GO) and Spirulina maxima (SM) algae was synthesized and applied to develop a preconcentration method based on the dispersive micro-solid phase extraction (D-μ-SPE) technique for the determination of Pb in water and infant beverages. In this work, Pb(II) was extracted with 3 mg of the hybrid bionanomaterial (GO@SM) followed by a back-extraction step using 500 µL of 0.6 mol L HCl. Then, a 1.5 × 10 mol L dithizone solution was added to the sample containing the analyte to form a purplish red-colored complex for its detection by UV-Vis spectrophotometry at 553 nm. An extraction efficiency of 98% was obtained after optimization of experimental variables such as GO@SM mass, pH, sample volume, type, and time of agitation. A detection limit of 1 μg L and a relative standard deviation of 3.5% (at 5 μg L Pb(II), n = 10) were achieved. The calibration linear range was obtained between 3.3 and 95 µg L Pb(II). The proposed method was successfully applied for the preconcentration and determination of Pb(II) in infant beverages. Finally, the greenness degree of the D-µ-SPE method was evaluated using the Analytical GREEnness calculator (AGREE), obtaining a score of 0.62.
一种新型的氧化石墨烯（GO）和螺旋藻（SM）藻类杂化仿生纳米材料被合成，并应用于开发一种基于分散微固相萃取（D-μ-SPE）技术的预浓缩方法，用于测定水中和婴儿饮料中的 Pb。在这项工作中，用 3mg 的杂化仿生纳米材料（GO@SM）提取 Pb(II)，然后用 500µL 0.6mol L HCl 进行反萃取。然后，将 1.5×10 mol L 二硫腙溶液加入含有分析物的样品中，形成紫色红色络合物，通过紫外可见分光光度法在 553nm 处检测。在优化实验变量（如 GO@SM 质量、pH、样品体积、搅拌类型和时间）后，获得了 98%的萃取效率。检测限为 1μg L，相对标准偏差为 3.5%（在 5μg L Pb(II)时，n=10）。校准线性范围为 3.3 至 95μg L Pb(II)。该方法成功应用于婴儿饮料中 Pb(II)的预浓缩和测定。最后，使用分析绿色度计算器（AGREE）评估 D-μ-SPE 方法的绿色度，得到 0.62 的分数。
