Centro de Quimica e Bioquimica e Centro de Quimica Estrutural, Faculdade de Ciências, Universidade de Lisboa, 1749-016 Lisboa, Portugal.
Centro de Quimica e Bioquimica e Centro de Quimica Estrutural, Faculdade de Ciências, Universidade de Lisboa, 1749-016 Lisboa, Portugal.
J Pharm Biomed Anal. 2018 May 10;153:126-134. doi: 10.1016/j.jpba.2018.02.001. Epub 2018 Feb 5.
The present contribution aims to design new-generation bar adsorptive microextraction (BAμE) devices that promote an innovative and much better user-friendly analytical approach. The novel BAμE devices were lab-made prepared having smaller dimensions by using flexible nylon-based supports (7.5 × 1.0 mm) coated with convenient sorbents (≈ 0.5 mg). This novel advance allows effective microextraction and back-extraction ('only single liquid desorption step') stages as well as interfacing enhancement with the instrumental systems dedicated for routine analysis. To evaluate the achievements of these improvements, four antidepressant agents (bupropion, citalopram, amitriptyline and trazodone) were used as model compounds in aqueous media combined with liquid chromatography (LC) systems. By using an N-vinylpyrrolidone based-polymer phase good selectivity and efficiency were obtained. Assays performed on 25 mL spiked aqueous samples, yielded average recoveries in between 67.8 ± 12.4% (bupropion) and 88.3 ± 12.1% (citalopram), under optimized experimental conditions. The analytical performance also showed convenient precision (RSD < 12%) and detection limits (50 ng L), as well as linear dynamic ranges (160-2000 ng L) with suitable determination coefficients (r > 0.9820). The application of the proposed analytical approach on biological fluids showed negligible matrix effects by using the standard addition methodology. From the data obtained, the new-generation BAμE devices presented herein provide an innovative and robust analytical cycle, are simple to prepare, cost-effective, user-friendly and compatible with the current LC autosampler systems. Furthermore, the novel devices were designed to be disposable and used together with negligible amounts of organic solvents (100 μL) during back-extraction, in compliance with the green analytical chemistry principles. In short, the new-generation BAμE devices showed to be an eco-user-friendly approach for trace analysis of priority compounds in biological fluids and a versatile alternative over other well-stablished sorption-based microextraction techniques.
本研究旨在设计新一代棒吸附微萃取（BAμE）装置，以促进创新和更友好的用户分析方法。新型 BAμE 装置采用柔性尼龙基支撑物（7.5×1.0mm）制成，尺寸更小，并涂有方便的吸附剂（≈0.5mg）。这种新型改进允许进行有效的微萃取和反萃取（“仅单步液体解吸”）阶段，以及与专用常规分析仪器系统的界面增强。为了评估这些改进的效果，使用四种抗抑郁药（安非他酮、西酞普兰、阿米替林和曲唑酮）作为模型化合物在水介质中与液相色谱（LC）系统结合使用。使用基于 N-乙烯基吡咯烷酮的聚合物相，获得了良好的选择性和效率。在优化实验条件下，对 25mL 加标水样进行测定，得到的平均回收率在 67.8±12.4%（安非他酮）和 88.3±12.1%（西酞普兰）之间。分析性能还表现出方便的精密度（RSD<12%）和检测限（50ng L），以及线性动态范围（160-2000ng L），合适的测定系数（r>0.9820）。使用标准添加法，在生物流体中的应用表明该分析方法具有可忽略的基质效应。从获得的数据来看，本文提出的新一代 BAμE 装置提供了一种创新且强大的分析周期，制备简单、经济高效、使用方便，并且与当前的 LC 自动进样器系统兼容。此外，新型装置设计为一次性使用，并在反萃取过程中使用少量有机溶剂（100μL），符合绿色分析化学原则。简而言之，新一代 BAμE 装置是一种用于痕量分析生物流体中优先化合物的生态友好型方法，是其他成熟的基于吸附的微萃取技术的多功能替代方法。
