Fan Haocheng, Tan Dongqin, Wang Yue, Li Yanying, Wang Degao
College of Environmental Science and Engineering, Dalian Maritime University, Dalian, Liaoning, China.
J Sep Sci. 2025 Jun;48(6):e70197. doi: 10.1002/jssc.70197.
Magnetic molecularly imprinted polymers (MMIPs) were synthesized by bulk polymerization using N-methylphenethylamine as a dummy template for selective extraction of four amphetamine-type stimulants (ATSs) in sewage and urine. The MMIPs were characterized by scanning electron microscopy, vibrating sample magnetometer, Fourier transform infrared spectroscopy and thermogravimetric analysis, revealing a porous structure (35-60 µm) with a saturation magnetization of 1.8 emu/g, enabling rapid magnetic separation within 1 min. Adsorption kinetics followed a pseudo-second-order model, achieving over 80% adsorption within 10 min and an imprinting factor of 2.4-3.3, demonstrating high selectivity for ATSs over structural analogs. Optimized magnetic solid-phase extraction (MSPE) conditions yielded recoveries over 81% with relative standard deviation (RSD) below 5.5%. Coupled with high performance liquid chromatography-tandem mass spectrometry, the proposed MMIPs-MSPE method exhibited a linear range of 1-100 ng/mL, low detection limits (5.2-19 ng/L), and quantification limits (17.0-65.0 ng/L). The pre-concentration factor of ATSs was 19.3-19.9. Successful application to real sewage and urine samples confirmed robust matrix interference resistance and reliability (recoveries: 82.1%-116%, RSD < 6.4%). This study provides a sensitive, reusable, and environmentally friendly approach for monitoring ATSs in environmental and forensic matrices.
以N-甲基苯乙胺为虚拟模板，通过本体聚合法合成了磁性分子印迹聚合物（MMIPs），用于选择性萃取污水和尿液中的四种苯丙胺类兴奋剂（ATSs）。通过扫描电子显微镜、振动样品磁强计、傅里叶变换红外光谱和热重分析对MMIPs进行了表征，结果表明其具有多孔结构（35 - 60 µm），饱和磁化强度为1.8 emu/g，能够在1分钟内实现快速磁分离。吸附动力学遵循准二级模型，在10分钟内吸附率超过80%，印迹因子为2.4 - 3.3，表明对ATSs的选择性高于结构类似物。优化后的磁性固相萃取（MSPE）条件下回收率超过81%，相对标准偏差（RSD）低于5.5%。结合高效液相色谱 - 串联质谱，所提出的MMIPs - MSPE方法线性范围为1 - 100 ng/mL，检测限低（5.2 - 19 ng/L），定量限为（17.0 - 65.0 ng/L）。ATSs的预富集因子为19.3 - 19.9。成功应用于实际污水和尿液样品，证实了其具有强大的抗基质干扰能力和可靠性（回收率：82.1% - 116%，RSD < 6.4%）。本研究为环境和法医基质中ATSs的监测提供了一种灵敏、可重复使用且环保的方法。
