Laboratory of Toxicant and Drug Analyses, Faculty of Pharmaceutical Sciences, Federal University of Alfenas, Alfenas, MG, 37130-001, Brazil.
Institute of Chemistry, Federal University of Alfenas, Alfenas, MG, 37130-001, Brazil.
Mikrochim Acta. 2024 Sep 25;191(10):620. doi: 10.1007/s00604-024-06698-2.
Magnetic particle spray mass spectrometry (MPS-MS), an innovative ambient ionization technique proposed by our research group, was employed to determine beta-blockers in human plasma samples. A dispersive solid phase extraction of atenolol, metoprolol, labetalol, propranolol, nadolol, and pindolol was carried out using magnetic molecularly imprinted polymer (M-MIP) particles that were attached to the tip of a metal probe, which was placed in the mass spectrometer inlet. A solvent (1% formic acid in methanol) was dispensed on the particles, and the Taylor cone was formed around them (in high voltage). The analytes were desorbed/ionized and determined by a triple quadrupole mass spectrometer. M-MIP was synthesized with oxprenolol as a pseudo-template, demonstrating good selectivity to beta-blockers compared with no-analog molecules, with an adsorption process occurring in monolayers, according to isotherm studies. Kinetic experiments indicated chemisorption as the predominant M-MIP/analyte interaction. The analytical curves were linear (R > 0.98), and the limit of quantification was 3 µg L for all the analytes. Limits of detection ranged from 0.64 to 2.41 µg L. Precisions (relative standard deviation) and accuracies (relative error) ranged from 3.95 to 21.20% and -17.05 to 18.93%, respectively. MPS-MS proved to be a simple, sensitive, and advantageous technique compared with conventional approaches. The analyses were fast, requiring no chromatographic separation and without ionic suppression. The method is aligned with green chemistry principles, requiring minimal sample, solvent, and sorbent amounts. MPS-MS successfully integrates sample preparation and ambient ionization mass spectrometry and holds great potential for application with other sorbents, samples, and analytes.
磁性粒子喷雾质谱(MPS-MS)是本研究团队提出的一种创新的环境电离技术,用于测定人血浆样品中的β受体阻滞剂。采用磁性分子印迹聚合物(M-MIP)颗粒作为分散固相萃取剂,对阿替洛尔、美托洛尔、拉贝洛尔、普萘洛尔、纳多洛尔和吲哚洛尔进行萃取,M-MIP 颗粒附着在金属探针的尖端,将探针置于质谱仪入口处。在颗粒上滴加溶剂(甲醇中的 1%甲酸),并在其周围形成泰勒锥(在高电压下)。分析物被解吸/离子化,并由三重四极杆质谱仪进行测定。以氧烯洛尔为模板分子合成 M-MIP,与非类似物分子相比,对β受体阻滞剂表现出良好的选择性,根据等温研究,吸附过程发生在单层中。动力学实验表明,化学吸附是 M-MIP/分析物相互作用的主要形式。分析曲线呈线性(R > 0.98),所有分析物的定量限均为 3 µg/L。检测限范围为 0.64 至 2.41 µg/L。精密度(相对标准偏差)和准确度(相对误差)范围分别为 3.95%至 21.20%和-17.05%至 18.93%。与传统方法相比,MPS-MS 被证明是一种简单、灵敏且有利的技术。分析速度快,无需色谱分离,且不存在离子抑制。该方法符合绿色化学原则,所需样品、溶剂和吸附剂的用量最少。MPS-MS 成功地将样品制备和环境电离质谱集成在一起,对于与其他吸附剂、样品和分析物的应用具有很大的潜力。