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New challenges in sample preparation: Miniaturized stir bar sorptive dispersive microextraction as a high-throughput and feasible approach for low-availability sample preparation
Analytica Chimica Acta ( IF 6.2 ) Pub Date : 2022-11-15 , DOI: 10.1016/j.aca.2022.340627
Cristian Azorín 1 , Juan L Benedé 1 , Alberto Chisvert 1
Affiliation  

The miniaturization of stir bar sorptive dispersive microextraction (mSBSDME) for the analysis of low-availability samples is presented. This new methodology is based on the principles of stir bar sorptive dispersive microextraction, but the amount of sorbent and, most importantly, the amount of sample are considerably reduced to a tiny amount and a few microliters, respectively. Thus, affordable 400-μL flat-base glass inserts and minute bar-shape neodymium magnets (3 mm length x 2 mm diameter) were used as extraction devices hold by a specifically designed multiextraction assembly, which comprises a high-rate stirring plate and a 3D-printed support to treat 15 samples simultaneously. This new approach allows a fast, affordable, portable, and high-throughput analysis of low-volume samples, expanding the potential of the technique. The same extraction device is used along the different stages, thus avoiding transfers, which reduces sample handling. Besides, the reduction in the sample, sorbent and organic solvent amounts allows a considerable decrease of the waste generation, and thus pursues a green sample preparation for bioanalysis. As a proof-of-concept of this new methodology, cortisone and cortisol were determined in human saliva using a composite material made of a reversed phase polymer (Strata™-X-RP) and CoFe2O4 magnetic nanoparticles. Liquid chromatography coupled to tandem mass spectrometry was used to measure both analytes obtaining good analytical features in terms of linearity (R2 > 0.997), method limits of detection and quantification (22.6 and 75.5 ng L−1 for cortisone, and 19.3 and 64.3 ng L−1 for cortisol, respectively), repeatability (RSD ≤11%) and relative recoveries (78–134%).



中文翻译:

样品制备的新挑战:微型搅拌棒吸附分散微萃取作为低可用性样品制备的高通量和可行方法

介绍了用于分析低可用性样品的搅拌棒吸附分散微萃取 (mSBSDME) 的小型化。这种新方法基于搅拌棒吸附分散微萃取的原理,但吸附剂的量和最重要的是样品量分别显着减少到极少量和几微升。因此,经济实惠的 400 μL 平底玻璃插入物和微小的棒形钕磁铁(3 毫米长 x 2 毫米直径)被用作由专门设计的多重萃取组件固定的萃取装置,该装置包括一个高速搅拌板和一个3D 打印支架可同时处理 15 个样品。这种新方法允许对少量样品进行快速、经济、便携和高通量的分析,从而扩展了该技术的潜力。不同阶段使用相同的提取设备,从而避免转移,从而减少样品处理。此外,样品、吸附剂和有机溶剂用量的减少使得废物的产生量大大减少,从而追求绿色的生物分析样品制备。作为这种新方法的概念验证,使用由反相聚合物 (Strata™-X-RP) 和 CoFe 制成的复合材料测定了人类唾液中的可的松和皮质醇2 O 4磁性纳米粒子。使用与串联质谱联用的液相色谱法测量两种分析物,在线性 (R 2  > 0.997)、检测和定量方法限度(可的松为 22.6 和 75.5 ng L -1,可的松为 19.3 和 64.3 ng )方面获得良好的分析特征皮质醇分别为L -1 )、重复性(RSD ≤11%)和相对回收率(78–134%)。

更新日期:2022-11-16
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