Tokalıoğlu Şerife, Demirişler Melike Selenay, Şahan Halil, Patat Şaban
Erciyes University, Faculty of Sciences, Chemistry Department, 38039, Kayseri, Turkey.
Kayseri University, Department of Basic Sciences of Engineering, 38280, Kayseri, Turkey.
Anal Methods. 2023 Nov 9;15(43):5846-5854. doi: 10.1039/d3ay01579c.
A fast and simple dispersive solid-phase microextraction method (d-SPμE) was described for the determination of copper and lead in food, water, and sediments using FAAS. Firstly, nanoflower AlO@carbon spheres composite (NF AlO@CSs) was synthesized and then characterized. The obtained NF AlO@CSs was used for the d-SPμE of copper and lead in aqueous solutions. The influence of important parameters like pH, contact time, eluent conditions, volume of sample, and competing ion effects on the d-SPμE efficiency of copper and lead was investigated. They were pH, 7; eluent, 2 mol L HCl (2 mL); sample volume, 250 mL for copper and 150 mL for lead with recoveries ≥90%. The adsorption and elution of analytes on NF AlO@CSs were realized quickly without vortexing. The LODs of the d-SPμE for copper and lead were found to be 0.69 μg L and 2.8 μg L, respectively, while its PF was 125 for copper and 75 for lead. The intra-day precision and inter-day repeatability (RSD%, = 7) were 1.3% and 1.6% for Cu(II) and 2.3% and 3.2% for Pb(II), respectively. Finally, the accuracy of the d-SPμE was investigated by determination of the analytes in four certified reference materials (TMDA-53.3 Lake water, NW-TMDA-54.6 Lake water, NIST 1573a Tomato leaves, and NIST RM 8704 Buffalo River Sediment). The analyte recoveries together with analyses of dam water, river water, wastewater, sea water, sumac, tea, chocolate, and lentils were studied. The results indicate that recoveries ranged from 90 to 103% in water samples and 91 to 110% in food samples.
描述了一种快速简便的分散固相微萃取方法（d-SPμE），用于使用火焰原子吸收光谱法（FAAS）测定食品、水和沉积物中的铜和铅。首先，合成了纳米花AlO@碳球复合材料（NF AlO@CSs），然后对其进行了表征。将所得的NF AlO@CSs用于水溶液中铜和铅的d-SPμE。研究了pH、接触时间、洗脱条件、样品体积和竞争离子效应等重要参数对铜和铅d-SPμE效率的影响。它们分别是pH为7；洗脱液为2 mol/L HCl（2 mL）；铜的样品体积为250 mL，铅的样品体积为150 mL，回收率≥90%。分析物在NF AlO@CSs上的吸附和洗脱无需涡旋即可快速实现。发现铜和铅的d-SPμE的检测限分别为0.69 μg/L和2.8 μg/L，而其富集因子铜为125，铅为75。Cu(II)的日内精密度和日间重复性（RSD%，n = 7）分别为1.3%和1.6%，Pb(II)的分别为2.3%和3.2%。最后，通过测定四种有证标准物质（TMDA-53.3湖水、NW-TMDA-54.6湖水、NIST 1573a番茄叶和NIST RM 8704布法罗河沉积物）中的分析物来研究d-SPμE的准确性。研究了分析物回收率以及对坝水、河水、废水、海水、漆树、茶、巧克力和小扁豆的分析。结果表明，水样中的回收率为90%至103%，食品样品中的回收率为91%至110%。
