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磁性表面印迹聚合物微球与 HPLC-MS/MS 联用检测水中的苯丙胺类毒品

Magnetic surface-imprinted polymer microspheres coupled with HPLC-MS/MS for sensitive detection of amphetamine-type drugs in water.

机构信息

College of Environmental Science and Engineering, Dalian Maritime University, No.1 Linghai Road, Dalian, 116026, China.

College of Environmental Science and Engineering, Dalian Maritime University, No.1 Linghai Road, Dalian, 116026, China.

出版信息

J Chromatogr A. 2024 Aug 16;1730:465097. doi: 10.1016/j.chroma.2024.465097. Epub 2024 Jun 15.

Abstract

Magnetic surface imprinted polymer microspheres (FeO@MIPs) were successfully synthesized via Pickering emulsion polymerization, utilizing N-Methylphenethylamine as a surrogate template for amphetamine-type drugs. FeO@MIPs not only possessed excellent dispersibility and enough magnetic properties in aqueous solutions, but also displayed good selectivity towards six amphetamines, with an imprinting factor ranging from 1.8 to 2.6. The adsorption kinetics closely aligned with the pseudo-second-order model, and the adsorption efficiency exceeds 80 % for each amphetamine at equilibrium. FeO@MIPs were then employed as the efficient adsorbents for the extraction of amphetamine drugs. Extraction parameters, including sample pH, the mass of adsorbent, and the type and volume of eluting solvent, were carefully optimized. In combination with the high performance liquid chromatography tandem triple quadrupole mass spectrometry (HPLC-MS/MS), a selective magnetic solid-phase extraction (MISPE) method utilizing FeO@MIPs was developed for the detection of six amphetamines in water samples. The limits of detection and limits of quantitation were determined to be 5.2∼23 ng L and 17∼77 ng L, respectively. Recoveries for the six target drugs from lake water and sewage samples fell within the range of 87.2∼110 %. Additionally, the MISPE-HPLC-MS/MS method exhibited excellent repeatability, with a precision below 8.5 % at two spiking levels. The prepared FeO@MIPs possessed the advantages of high selectivity, straightforward preparation, facile separation and good reusability, and was highly suitable for the efficient extraction of amphetamine-type substances in complex environmental water.

摘要

磁性表面印迹聚合物微球(FeO@MIPs)通过 Pickering 乳液聚合成功合成,利用 N-甲基苯乙胺作为苯丙胺类药物的替代模板。FeO@MIPs 不仅在水溶液中具有良好的分散性和足够的磁性,而且对六种苯丙胺类药物具有良好的选择性,印迹因子范围为 1.8 至 2.6。吸附动力学与拟二级模型密切吻合,每种苯丙胺在平衡时的吸附效率均超过 80%。然后,将 FeO@MIPs 用作提取苯丙胺类药物的有效吸附剂。仔细优化了包括样品 pH 值、吸附剂质量以及洗脱溶剂类型和体积在内的提取参数。结合高效液相色谱串联三重四极杆质谱(HPLC-MS/MS),开发了一种基于 FeO@MIPs 的选择性磁固相萃取(MISPE)方法,用于检测水样中的六种苯丙胺类药物。检测限和定量限分别为 5.2∼23 ng L 和 17∼77 ng L。从湖水和污水样品中回收六种目标药物的回收率在 87.2∼110 %范围内。此外,MISPE-HPLC-MS/MS 方法表现出良好的重现性,在两个加标水平下精度低于 8.5 %。制备的 FeO@MIPs 具有高选择性、制备简单、易于分离和良好的可重复使用性等优点,非常适合从复杂环境水样中高效提取苯丙胺类物质。

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