Kwasnik Mark, Fuhrer Katrin, Gonin Marc, Barbeau Katherine, Fernandez Facundo M
School of Chemistry and Biochemistry, Georgia Institute of Technology, Atlanta, Georgia 30332, USA.
Anal Chem. 2007 Oct 15;79(20):7782-91. doi: 10.1021/ac071226o. Epub 2007 Sep 14.
In this article, we describe and characterize a novel ion mobility spectrometer constructed with monolithic resistive glass desolvation and drift regions. This instrument is equipped with switchable corona discharge and nanoelectrospray ionization sources and a Faraday plate detector. Following description of the instrument, pulsing electronics, and data acquisition system, we examine the effects of drift gas flow rate and temperature, and of the aperture grid to anode distance on the observed resolving power and sensitivity. Once optimum experimental parameters are identified, different ion gate pulse lengths, and their effect on the temporal spread of the ion packet were investigated. Resolving power ranged from an average value of 50 ms/ms for a 400-micros ion gate pulse, up to an average value of 68 ms/ms for a 100-micros ion gate pulse, and a 26-cm drift tube operated at 383 V cm(-1). Following these experiments, the radial distribution of ions in the drift region of the spectrometer was studied by using anodes of varying sizes, showing that the highest ionic density was located at the center of the drift tube. Finally, we demonstrate the applicability of this instrument to the study of small molecules of environmental relevance by analyzing a commercially available siderophore, deferoxamine mesylate, in both the free ligand and Fe-bound forms. Ion mobility experiments showed a dramatic shift to shorter drift times caused by conformational changes upon metal binding, in agreement with previous reversed-phase liquid chromatography observations.
在本文中,我们描述并表征了一种采用整体式电阻玻璃去溶剂化和漂移区构建的新型离子迁移谱仪。该仪器配备了可切换的电晕放电和纳米电喷雾电离源以及法拉第板探测器。在介绍了仪器、脉冲电子学和数据采集系统之后,我们研究了漂移气体流速和温度以及孔径栅极到阳极距离对观察到的分辨能力和灵敏度的影响。一旦确定了最佳实验参数,就研究了不同的离子门脉冲长度及其对离子包时间展宽的影响。在383 V cm⁻¹的电压下,对于一个400微秒的离子门脉冲,分辨能力的平均值为50 ms/ms,对于一个100微秒的离子门脉冲,分辨能力的平均值为68 ms/ms,漂移管长度为26厘米。在这些实验之后,通过使用不同尺寸的阳极研究了谱仪漂移区中离子的径向分布,结果表明最高离子密度位于漂移管的中心。最后,我们通过分析市售的铁载体甲磺酸去铁胺的游离配体形式和铁结合形式,证明了该仪器在研究与环境相关的小分子方面的适用性。离子迁移实验表明,金属结合后构象变化导致漂移时间显著缩短,这与之前反相液相色谱的观察结果一致。