Department of Chemistry, Shahid Bahonar University of Kerman, Kerman, Iran.
Department of Chemistry, Shahid Bahonar University of Kerman, Kerman, Iran.
Food Chem. 2019 Jul 30;287:382-389. doi: 10.1016/j.foodchem.2019.02.112. Epub 2019 Mar 2.
A magnetic solid-phase extraction method was developed using maghemite as an efficient sorbent for the separation and preconcentration of antimony prior to its determination by ET-AAS. Maghemite was synthesized through a simple method and characterized by XRD, FT-IR and SEM. Various factors affecting maghemite synthesis, separation and preconcentration of antimony such as desorption solvent type, concentration and volume, desorption temperature and time, sample pH, amount of sorbent, and extraction temperature and time were optimized. The effects of interfering ions were also investigated. Under optimized conditions, the method exhibited good linearity (r > 0.9960). The sorption capacity and enrichment factor (EF) of the method were 37.5 mg g and 242, respectively. The limit of detection (LOD) was 0.03 ng mL. The intraday, interday, and batch-to-batch relative standard deviations (%RSDs) were quite reasonable. The proposed method was applied to various real samples and the relative recoveries found were between 95.8 and 104.0 %.
采用磁固相萃取法，以磁赤铁矿为高效吸附剂，在 ET-AAS 测定前分离和预浓缩锑。通过简单的方法合成了磁赤铁矿，并通过 XRD、FT-IR 和 SEM 进行了表征。优化了影响磁赤铁矿合成、分离和预浓缩锑的各种因素，如解吸溶剂类型、浓度和体积、解吸温度和时间、样品 pH 值、吸附剂用量以及萃取温度和时间。还研究了干扰离子的影响。在优化条件下，该方法表现出良好的线性（r>0.9960）。该方法的吸附容量和富集因子（EF）分别为 37.5mg g 和 242。检测限（LOD）为 0.03ng mL。日内、日间和批间相对标准偏差（%RSD）相当合理。该方法已应用于各种实际样品，发现的相对回收率在 95.8%至 104.0%之间。
