A rapid and sensitive method for analyzing trace β-blockers in complex biological samples, which involved magnetic solid-phase extraction (MSPE) coupled with Fourier transform ion cyclotron resonance mass spectrometry (FTICR-MS), was developed. Novel nanosilver-functionalized magnetic nanoparticles with an interlayer of poly(3,4-dihydroxyphenylalanine) (polyDOPA@Ag-MNPs) were synthesized and used as MSPE adsorbents to extract trace β-blockers from biological samples. After extraction, the analytes loaded on the polyDOPA@Ag-MNPs were desorbed using an organic solvent and analyzed by FTICR-MS. The method was rapid and sensitive, with a total detection procedure of less than 10 min as well as limits of detection and quantification in the ranges of 3.5–6.8 pg/mL and 11.7–22.8 pg/mL, respectively. The accuracy of the method was also desirable, with recoveries ranging from 80.9% to 91.0% following the detection of analytes in human blood samples. All the experimental results demonstrated that the developed MSPE-FTICR-MS method was suitable for the rapid and sensitive analysis of trace β-blockers in complex biological samples.

开发了一种快速、灵敏地分析复杂生物样品中痕量 β 受体阻滞剂的方法，该方法包括磁固相萃取 (MSPE) 与傅里叶变换离子回旋共振质谱 (FTICR-MS) 相结合。合成了具有中间层聚 (3,4-二羟基苯丙氨酸) (polyDOPA@Ag-MNPs) 的新型纳米银功能化磁性纳米粒子，并将其用作 MSPE 吸附剂，以从生物样品中提取痕量 β-受体阻滞剂。萃取后，负载在 polyDOPA@Ag-MNPs 上的分析物使用有机溶剂解吸，并通过 FTICR-MS 进行分析。该方法快速灵敏，总检测过程不到 10 分钟，检测限和定量限分别在 3.5–6.8 pg/mL 和 11.7–22.8 pg/mL 范围内。该方法的准确性也很理想，在检测人体血液样本中的分析物后，回收率从 80.9% 到 91.0% 不等。所有实验结果表明，所开发的MSPE-FTICR-MS方法适用于复杂生物样品中痕量β受体阻滞剂的快速灵敏分析。