Ministry of Education Key Laboratory of Analytical Science for Food Safety and Biology, Fujian Provincial Key Laboratory of Analysis and Detection Technology for Food Safety, College of Chemistry, Fuzhou University, Fuzhou, Fujian 350116, China.
Fujian Vocational College of Bioengineering, Fuzhou, Fujian 350002, China.
Talanta. 2018 May 1;181:296-304. doi: 10.1016/j.talanta.2018.01.036. Epub 2018 Feb 3.
Core-shell structured magnetic covalent organic framework (FeO@COF) nanocomposites were synthesized via a facile approach at room temperature and explored as an absorbent for magnetic solid-phase extraction (MSPE) of bisphenols (BPs) from human serum sample. The as-prepared FeO@COF nanocomposites with core-shell structure possessed high specific surface area (181.36m/g), uniform mesoporous size (~ 3.6nm), high saturation magnetization (42.7emu/g), and excellent thermal and chemical stability, rendering it as an ideal adsorbent with high adsorption efficiency and size selectivity. The experimental parameters influencing extraction efficiency, including adsorbent dosage, extraction time, pH and ion strength, desorption solvent and time, were investigated in detail. Taking these advantages together, a simple, fast, effective and sensitive method that MPSE followed by HPLC-MS, was proposed to detect five BPs, which exhibited good linearity (r > 0.9982) within the concentration ranges of 0.1-50μg/L. Moreover, the low detection limits (1.0-78.1ng/L), signal-to-noise ratio (S/N = 3), the high enrichment factors (56-95 fold), and good recoveries (93.0-107.8%) with relative standard deviations (RSDs) less than 3.4% for inter-day and 6.9% for intra-day were achieved. The developed method was also successfully applied to the analysis of trace BPs in human serum sample, which demonstrated the most promising potential of the FeO@COF nanocomposites as good adsorbent in sample pretreatment.
核壳结构磁性共价有机框架（FeO@COF）纳米复合材料是通过在室温下的简便方法合成的，并作为从人血清样品中磁性固相萃取（MSPE）双酚（BP）的吸附剂进行了探索。所制备的具有核壳结构的 FeO@COF 纳米复合材料具有高比表面积（181.36m/g）、均匀的中孔尺寸（~3.6nm）、高饱和磁化强度（42.7emu/g）和优异的热稳定性和化学稳定性，使其成为具有高吸附效率和尺寸选择性的理想吸附剂。详细研究了影响萃取效率的实验参数，包括吸附剂用量、萃取时间、pH 值和离子强度、解吸溶剂和时间。综合这些优点，提出了一种简单、快速、有效和灵敏的方法，即 MPSE 后 HPLC-MS，用于检测五种 BP，其在 0.1-50μg/L 的浓度范围内表现出良好的线性（r>0.9982）。此外，还实现了低检测限（1.0-78.1ng/L）、信噪比（S/N=3）、高富集因子（56-95 倍）和良好的回收率（93.0-107.8%），日内 RSD 小于 3.4%，日间 RSD 小于 6.9%。该方法还成功应用于人血清样品中痕量 BP 的分析，证明了 FeO@COF 纳米复合材料作为样品预处理中良好吸附剂的最有前途的潜力。
