Lin Shumin, Liang Bolong, Zhao Zhe, Li Zhenqiu, Deng Kai, He Hongbin, Liang Shu-Xuan
Key Laboratory of Analytical Science and Technology of Hebei Province, State Key Laboratory of New Pharmaceutical Preparations and Excipients, College of Chemistry and Materials Science, Hebei University, Baoding 071002, PR China; Analysis and Testing Center, Inner Mongolia University of Science and Technology, Baotou 014010, China.
School of Eco-Environment, Hebei University, Baoding 071002, PR China.
J Chromatogr A. 2023 Oct 25;1709:464403. doi: 10.1016/j.chroma.2023.464403. Epub 2023 Sep 20.
Effective capture of quinolones (QNs) in animal-derived food is a vital procedure for food safety monitoring. However, the lack of adsorption specificity and difficult to recycle in complex substrate conditions have been major problems for most of the adsorbents. In this work, a magnetic FeO/MOF/COF composite (named FeO@NH-MIL-125@TpPa-SOH) was successfully synthesized with good magnetic responsiveness and conspicuous affinity towards QNs. The FeO/MOF/COF composite was used as a magnetic solid-phase extraction (MSPE) adsorbent for pretreatment and determination of QNs in meat samples. Under optimal MSPE conditions in combination with high performance liquid chromatography-quadrupole orbitrap high resolution mass spectrometer (HPLC-Q-Orbitrap HRMS), the proposed method had good linearity (R ≥ 0.9978) from 0.01 to 100ng g, low limits of detection (0.0016 to 0.0940ng g), good precision with relative standard deviations lower than 5.8%. This method was effectively applied to the detection of 17 QNs in the spiked pork, chicken and beef samples with satisfactory recoveries from 83.9 to 106.2%. The separation selectivity mainly due to the π-π interaction, hydrogen bonding, and electrostatic attraction between QNs and the sulfonic acid and amino functional groups of the composite. After verification, the stability and reusability of the composite meet the requirements of complex matrix sample pretreatment. The developed MSPE method based on the magnetic FeO/MOF/COF composite provided an ideal sample pretreatment alternative for determining trace QNs in complex matrixes with selectivity, simplicity, rapidity, and efficiency.
有效捕获动物源食品中的喹诺酮类药物（QNs）是食品安全监测的重要环节。然而，大多数吸附剂在复杂基质条件下缺乏吸附特异性且难以回收利用，这一直是主要问题。在本研究中，成功合成了一种具有良好磁响应性且对QNs具有显著亲和力的磁性FeO/MOF/COF复合材料（命名为FeO@NH-MIL-125@TpPa-SOH）。该FeO/MOF/COF复合材料用作磁性固相萃取（MSPE）吸附剂，用于肉类样品中QNs的预处理和测定。在最佳MSPE条件下结合高效液相色谱-四极杆轨道阱高分辨率质谱仪（HPLC-Q-Orbitrap HRMS），所提出的方法在0.01至100ng/g范围内具有良好的线性（R≥0.9978），检测限低（0.0016至0.0940ng/g），精密度良好，相对标准偏差低于5.8%。该方法有效地应用于加标猪肉、鸡肉和牛肉样品中17种QNs的检测，回收率令人满意，为83.9%至106.2%。分离选择性主要归因于QNs与复合材料的磺酸和氨基官能团之间的π-π相互作用、氢键和静电吸引。经验证，该复合材料的稳定性和可重复使用性满足复杂基质样品预处理的要求。基于磁性FeO/MOF/COF复合材料开发的MSPE方法为选择性、简便、快速、高效地测定复杂基质中的痕量QNs提供了一种理想的样品预处理方法。
