Schwieger Julius, Welters Klaus, Thoben Christian, Nitschke Alexander, Zimmermann Stefan, Belder Detlev
Institute of Analytical Chemistry, Leipzig University, Linnéstraße 3, Leipzig 04103, Germany.
Institute of Electrical Engineering and Measurement Technology, Leibniz University Hannover, Appelstraße 9a, Hannover 30167, Germany.
Anal Chem. 2025 Apr 15;97(14):7954-7960. doi: 10.1021/acs.analchem.5c00227. Epub 2025 Apr 5.
This study presents the first coupling of miniaturized chip-based supercritical fluid chromatography (SFC) with ion mobility spectrometry (IMS) enabling rapid two-dimensional analysis of moderately polar compounds. For the first time, ionization and analyte transfer at the SFC-IMS interface are achieved solely through eluent decompression in conjunction with a shifted electric IMS inlet potential. This straightforward approach significantly reduces instrumentation complexity and size, promoting system compactness and robustness. The integration of chip-based SFC with IMS enables high-speed separations of complex samples, drastically reducing analysis time while utilizing a detector capable of delivering structural information at a rapid acquisition rate and low cost. Evaluation of the SFC-IMS system as demonstrated through the chiral separation of Tröger's base revealed exceptional repeatability and sensitivity. Short columns and high flow rates resulted in record-speed SFC-IMS analysis in just six seconds. The system was successfully used to analyze a complex mixture containing five isomers, including naloxone and 6-monoacetylmorphine, in just 30 s.
本研究首次将基于芯片的微型超临界流体色谱(SFC)与离子迁移谱(IMS)联用,实现了对中等极性化合物的快速二维分析。首次仅通过洗脱液减压并结合移动的电IMS入口电位,实现了SFC-IMS接口处的离子化和分析物转移。这种直接的方法显著降低了仪器的复杂性和尺寸,提高了系统的紧凑性和稳健性。基于芯片的SFC与IMS的集成能够对复杂样品进行高速分离,在利用能够以快速采集速率和低成本提供结构信息的检测器的同时,大幅缩短分析时间。通过曲格列酮碱的手性分离对SFC-IMS系统进行评估,结果显示出卓越的重复性和灵敏度。短柱和高流速使得SFC-IMS分析在短短6秒内达到创纪录的速度。该系统成功用于在仅30秒内分析含有五种异构体(包括纳洛酮和6-单乙酰吗啡)的复杂混合物。