Department of Chemistry, Faculty of Science, University of Tehran, Tehran, Iran; Doctoral School of Science and Technology, Research Platform for Environmental Science (PRASE), Lebanese University, Lebanon.
Department of Chemistry, Faculty of Science, University of Tehran, Tehran, Iran.
J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Aug 15;1092:480-488. doi: 10.1016/j.jchromb.2018.06.049. Epub 2018 Jun 23.
A novel analytical method namely magnetic solid phase extraction in tandem with dispersive liquid-liquid microextraction was developed and used for the extraction/preconcentration of tetracycline (TCN), oxytetracycline (OTC) and doxycycline (DC) from bovine milk sample before HPLC-UV analysis. The β-cyclodextrin functionalized silica-coated magnetic graphene oxide (FeO@SiO@GO-β-CD) was used as an adsorbent. The adsorbent was fully characterized using FT-IR, SEM, EDX and Zeta potential techniques. The effective parameters on the performance of the method such as extraction solvent type and volume, adsorbent amount, desorption solvent type and volume, disperser solvent type, desorption time, ionic strength and pH value were investigated. The limit of detection (LOD) and limit of quantification (LOQ) were obtained in the ranges of 1.8-2.9 μg L and 6.1-9.7 μg L, respectively. The linearity was in the range of 10.0-200.0 μg L with satisfactory determination coefficients (R) higher than 0.9929 and a good precision (RSD < 8.8%). The recovery percentages for the analytes in real samples (bovine milk and water) were achieved in a range from 70.6 to 121.5%.
建立了一种新型分析方法，即磁固相萃取与分散液液微萃取串联，用于高效液相色谱-紫外分析前从牛奶奶样中提取/预浓缩四环素（TCN）、土霉素（OTC）和强力霉素（DC）。β-环糊精功能化的硅烷化磁性氧化石墨烯（FeO@SiO@GO-β-CD）被用作吸附剂。采用 FT-IR、SEM、EDX 和 Zeta 电位技术对吸附剂进行了全面表征。考察了萃取溶剂类型和体积、吸附剂用量、解吸溶剂类型和体积、分散剂溶剂类型、解吸时间、离子强度和 pH 值等因素对方法性能的影响。检测限（LOD）和定量限（LOQ）分别在 1.8-2.9μg/L 和 6.1-9.7μg/L 的范围内。线性范围为 10.0-200.0μg/L，相关系数（R）高于 0.9929，精密度良好（RSD<8.8%）。在实际样品（牛奶和水）中的回收率在 70.6%至 121.5%之间。
