School of Food and Biological Engineering, Shaanxi University of Science and Technology, Xi'an, 710021, China.
Key Laboratory of Life-Organic Analysis of Shandong Province, Qufu Normal University, Qufu, 273165, China.
Rapid Commun Mass Spectrom. 2020 May 30;34(10):e8742. doi: 10.1002/rcm.8742.
Sedatives, which are prone to cause residues in animals, have been abused in modern animal husbandry. Long-term consumption of contaminated meat products would be unfavorable to the human nervous system. Taking into account public health and food safety, it was essential to develop an effective method for the enrichment and detection of sedatives in meat.
Fe O @TbBd@ZIF-8 composites were synthesized by using Fe O nanoparticles as a magnetic core and 1,3,5-triformylbenzene (Tb) and benzidine (Bd) as two building blocks to form Fe O @TbBd. Furthermore, the zeolitic imidazolate framework-8 (ZIF-8) was modified on the surface of the Fe O @TbBd. In addition, Fe O @TbBd@ZIF-8 was used as a magnetic solid-phase extraction (MSPE) adsorbent of typical animal sedatives in pork samples. Mass spectrometry analysis was conducted by electrospray ionization triple-quadrupole mass spectrometry in positive-ion multiple reaction monitoring mode.
By combining the optimized MSPE approach with high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS), an accurate and sensitive method for the determination of sedatives was developed. The method exhibited good linearity in the range of 0.03-70 μg/kg with the correlation coefficient (R ) ranging from 0.9982 to 0.9999, high sensitivity with limits of detection (LODs) ranging from 0.04 to 0.2 μg/kg, and high precision with relative standard deviation (RSD) less than 5.5%. The adsorption behaviors of Fe O @TbBd@ZIF-8 towards sedatives were more suitably described by a pseudo-second-order kinetic and Freundlich isotherm model.
The proposed MSPE-HPLC/MS/MS method was successfully applied to the determination of sedatives in real samples and showed excellent applicability. Several sedatives were detected in the selected meat samples. The developed method was shown to be facile, sensitive and accurate for sedative detection and also showed great prospects for determination of sedatives from other complex samples.
镇静剂容易在动物体内残留，已在现代畜牧业中被滥用。长期食用受污染的肉类产品不利于人类的神经系统。考虑到公共卫生和食品安全，开发一种有效的方法来富集和检测肉类中的镇静剂至关重要。
通过以 FeO 纳米颗粒为磁核，以 1,3,5-均苯三甲酰氯（Tb）和联苯胺（Bd）为两个构筑块，合成了 FeO@TbBd@ZIF-8 复合材料。进一步在 FeO@TbBd 的表面修饰沸石咪唑酯骨架-8（ZIF-8）。此外，将 FeO@TbBd@ZIF-8 用作猪肉样品中典型动物镇静剂的磁性固相萃取（MSPE）吸附剂。通过电喷雾电离三重四极杆质谱在正离子多反应监测模式下进行质谱分析。
通过将优化的 MSPE 方法与高效液相色谱/串联质谱（HPLC/MS/MS）相结合，开发了一种用于测定镇静剂的准确灵敏的方法。该方法在 0.03-70μg/kg 范围内表现出良好的线性关系，相关系数（R）范围为 0.9982-0.9999，灵敏度高，检出限（LOD）范围为 0.04-0.2μg/kg，精密度高，相对标准偏差（RSD）小于 5.5%。FeO@TbBd@ZIF-8 对镇静剂的吸附行为更适合用准二级动力学和 Freundlich 等温模型来描述。
所提出的 MSPE-HPLC/MS/MS 方法成功应用于实际样品中镇静剂的测定，具有良好的适用性。在选定的肉样中检测到几种镇静剂。该方法简便、灵敏、准确，适用于镇静剂的检测，对于从其他复杂样品中检测镇静剂也具有广阔的前景。
