A simple magnetic dispersive solid-phase extraction (MDSPE) methodology based on mesoporous Fe₃O₄@ succinic acid nanospheres and high‐performance liquid chromatography–tandem mass spectrometry (HPLC‐MS/MS) has been developed to determine kanamycin (KNM) and neomycin (NEO) contents in Measles, Mumps, and Rubella (MMR) vaccine products. The monodispersed mesoporous Fe₃O₄ nanospheres with self-assembled carboxyl terminated shell have been prepared via a simple solvothermal method. These as-synthesized mesoporous Fe₃O₄ nanospheres showed a high magnetic saturation value (M_s = 46 emu g⁻¹) and large specific surface area (111.12 m² g⁻¹) which made them potential candidates as sorbents in magnetic solid-phase extraction. The adsorption experimental data fitted well with the Freundlich-Langmuir isotherm and followed a pseudo-second-order kinetic model. Moreover influential parameters on extraction efficiency were investigated and optimized. Under optimal conditions, the limits of detection for KNM and NEO were 1.0 and 0.1 ng mL⁻¹, respectively. Recovery assessments using real samples exhibited recoveries in the range of 96.0 ± 4.3 to 101.5 ± 7.1 %, with relative standard deviations of <10.7% (for intra- day) and <14.6% (for inter- day). The proposed method was successfully applied for different spiked and un-spiked MMR vaccine samples. The presented extraction method provides a fast, selective, robust and practical platform for the detection of KNM and NEO in MMR vaccine samples.

已经开发了一种基于介孔Fe ₃ O ₄ @琥珀酸纳米球和高效液相色谱-串联质谱（HPLC-MS / MS）的简单磁分散固相萃取（MDSPE）方法来测定卡那霉素（KNM）和麻疹，腮腺炎和风疹（MMR）疫苗产品中的新霉素（NEO）含量。采用简单的溶剂热法制备了具有自组装羧基端壳的单分散介孔Fe ₃ O ₄纳米球。这些合成的介孔Fe ₃ O ₄纳米球显示出高的磁饱和值（M _s  = 46 emu g ^-1）和较大的比表面积（111.12 m ² g ^-1），这使其成为磁性固相萃取中潜在的吸附剂。吸附实验数据与Freundlich-Langmuir等温线非常吻合，并遵循伪二级动力学模型。研究并优化了影响提取效率的参数。在最佳条件下，KNM和NEO的检出限为1.0和0.1 ng mL ^-1， 分别。使用实际样品进行的回收率评估显示回收率在96.0±4.3至101.5±7.1％的范围内，相对标准偏差分别为<10.7％（对于日内）和<14.6％（对于日间）。该方法成功应用于不同加标和未加标的MMR疫苗样品。提出的提取方法为检测MMR疫苗样品中的KNM和NEO提供了一种快速，选择性，鲁棒和实用的平台。