A method of combining magnetic solid-phase separation (MSPE) and chiral capillary electrophoresis (CE) is developed for enantioseparation of trace amounts of β-blockers. Polynorepinephrine-functionalized magnetic nanoparticles (polyNE-MNPs) are synthesized and applied to simultaneously extract three β-blockers (carteolol, metoprolol, and betaxolol). The prepared polyNE-MNPs are spherical with a diameter of 198 ± 17 nm and the thickness of the polyNE coating is about 14 nm. PolyNE possesses abundant catechol hydroxyl and secondary amine groups, endowing the MNPs with excellent hydrophilicity. Under the optimum conditions, the extraction efficiencies of polyNE-MNPs for β-blockers are in the range of 89.6 to 100%, with relative standard deviations (RSDs) below 3.5%. The extraction process can be finished in 4 min. Field-enhanced sample injection (FESI) in chiral CE is constructed to further enhance the sensitivities of β-blocker enantiomers. The limits of detection for β-blocker enantiomers by the FESI-CE with polyNE-MNPs are in the range of 0.401 to 1.59 ng mL⁻¹. The practicability of this method in real samples is evaluated by analysis of human urine samples. The recoveries for each enantiomer of β-blockers in the real samples range from 89.5 to 92.8%, with RSDs ranging from 0.37 to 5.9%. The whole detection process can be finished in less than 0.5 h. The method demonstrates its great potential in the pharmacokinetic and pharmacodynamic studies of chiral drugs in humans.

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开发了一种将磁性固相分离（MSPE）与手性毛细管电泳（CE）结合的方法，用于对映体分离痕量的β-阻滞剂。合成了聚去甲肾上腺素功能化的磁性纳米颗粒（polyNE-MNPs），并用于同时提取三种β-受体阻滞剂（胡萝卜素，美托洛尔和紫杉醇）。制备的polyNE-MNP是球形的，直径为198±17nm，并且polyNE涂层的厚度为约14nm。PolyNE具有丰富的儿茶酚羟基和仲胺基，赋予MNP极好的亲水性。在最佳条件下，polyNE-MNP对β受体阻滞剂的提取效率在89.6至100％的范围内，相对标准偏差（RSD）低于3.5％。提取过程可以在4分钟内完成。手性CE中的场增强样品注射（FESI）可以进一步增强β受体阻滞剂对映体的敏感性。FESI-CE和polyNE-MNP对β受体阻滞剂对映体的检出限为0.401至1.59 ng mL^-1。该方法在实际样品中的实用性通过对人类尿液样品的分析进行评估。实际样品中每种β-阻滞剂对映体的回收率在89.5至92.8％之间，RSD在0.37至5.9％之间。整个检测过程可以在不到0.5小时的时间内完成。该方法在手性药物在人体的药代动力学和药效学研究中显示出巨大的潜力。

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