Ion mobility spectrometry after supercritical fluid chromatography.

Ion mobility spectrometry after supercritical fluid chromatography.
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超临界流体色谱后的离子迁移谱测定。

DOI:
10.1021/ac00128a004
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发表时间:
1987
影响因子:
7.4
通讯作者:
HillJr,HH
HillJr,HH
中科院分区:
化学1区
文献类型:
--
作者:
Rokushika,S;Hatano,H;HillJr,HH

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建立了具有柱上紫外吸收检测和常压离子迁移谱的毛细管超临界流体色谱仪。本文用一系列苯甲酸酯和甲酯作了初步实验,以测定超临界流体色谱(SFC)和离子迁移光谱(IMS)的基本相容性。通过使用CO2作为色谱移动的相和离子迁移率漂移气体来完成毛细管SFC后的IMS。在适当的色谱保留时间下的离子迁移率扫描产生了每种供试化合物的可重现和独特的光谱。采用这种特殊的设计,观察到明显的清除时间问题,在整个色谱运行过程中产生严重的溶剂污染,并将这种设计限制在检测较低分子量化合物。尽管如此,在CO2中离子迁移率谱的成功产生,离子迁移率检测相对于“柱上”UV吸收检测的增强的灵敏度,毛细管超临界流体色谱(SFC)用于低温分离化合物的应用在过去几年中得到了显著的发展(1、第2段)。二氧化碳在相对温和的条件下成为超临界流体,已被发现是SFC的特别方便的移动的相。其相对高的极化率提供了比这种非极性化合物可能预期的更好的溶剂化特性,而其高电离电位和惰性特性使其理想地适合于与通常与气相色谱一起使用的灵敏的环境压力电离检测器连接。火焰离子化检测器是SFC的主要离子化检测方法,但也研究了其他离子化检测器(3-5)。
A capillary supercritical fluid chromatograph with on-column UV absorption detection and ambient pressure Ion mobility spectrometry was constructed. Preliminary experiments using a series of benzoate and methyl esters were conducted to determine the basic compatabWty of supercritical fluid chro-matography (SFC) and Ion mobWy spectrometry (IMS). IMS after capillary SFC was accomplished by using COa as both the chromatographic mobile phase and the Ion mobility drift gas. Ion mobility scans at appropriate chromatographic re-tention times produced reproducible and distinct spectra for each of the test compounds. With this particular design, significant clearance time problems were observed, creating serious solvent contamination throughout the chromatographic run and limiting this design to the detection of lower molecular weight compounds. Nevertheless, the successful production of Ion mobWty spectra In COa, the enhanced sensitivity of Ion mobility detection over “on-column” UV absorption detection, and the ease with which the Interface can be achieved dem-onstrated that the combination of SFC with IMS deserves further attention.The use of capillary supercritical fluid chromatography (SFC) for low-temperature separation of compounds has ex-panded significantly over the last few years (1, 2). Carbon dioxide, which becomes a supercritical fluid under relatively mild conditions, has been found to be an especially convenient mobile phase for SFC. Its relatively high polarizability pro-vides better solvating characteristics than might be expected for such a nonpolar compound, while its high ionization po-tential and inert character make it ideally suited for interfacing with sensitive ambient-pressure ionization detectors commonly used with gas chromatography. Flame ionization detectors have been the primary ionization detection method of choice with SFC, but other ionization detectors havealso been investigated (3-5).
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