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一种超快速气相色谱仪与具有高重复率和流量优化离子源的离子淌度谱仪联用,以解析短色谱峰。

A hyper-fast gas chromatograph coupled to an ion mobility spectrometer with high repetition rate and flow-optimized ion source to resolve the short chromatographic peaks.

机构信息

Leibniz Universität Hannover, Institute of Electrical Engineering and Measurement Technology, Department of Sensors and Measurement Technology, Hannover 30167, Germany.

Leibniz Universität Hannover, Institute of Electrical Engineering and Measurement Technology, Department of Sensors and Measurement Technology, Hannover 30167, Germany.

出版信息

J Chromatogr A. 2024 Nov 8;1736:465376. doi: 10.1016/j.chroma.2024.465376. Epub 2024 Sep 12.

DOI:10.1016/j.chroma.2024.465376
PMID:39277980
Abstract

By combining the high selectivity of a gas chromatograph (GC) with the high sensitivity and decent selectivity of an ion mobility spectrometer (IMS), GC-IMS have become increasingly popular in many applications. However, most GC suffer from long analysis times. In contrast, an hyper-fast GC allows for extremely fast analysis in the tens of seconds while reaching comparably high resolution. In turn, coupling such hyper-fast GC with IMS requires sufficiently high repetition rate of recording full IMS spectra to resolve the short GC peaks. Therefore, we present a drift tube IMS with 100 Hz repetition rate. Key is a small effective detector volume combined with short drift length. Therefore, the ion source of the IMS combines a small reaction region with an extended field-switching ion shutter and optimized gas flows. To resolve even the shortest GC peaks with a full width at half maximum of 100 ms, a short drift length of just 41 mm was used, achieving a measurement time of 10 ms per spectrum and hence ten data points across the shortest GC peak. To avoid condensation of the sample, the entire IMS was heated isothermally to 120 °C. Despite short drift times and high temperatures, the IMS still reaches high resolving power of R = 60. The hyper-fast GC-IMS reaches low detection limits in the low ppb range. For demonstration, ketone mixes and three different hop varieties were analyzed in <30 s.

摘要

通过将气相色谱仪(GC)的高选择性与离子迁移谱仪(IMS)的高灵敏度和良好的选择性相结合,GC-IMS 在许多应用中变得越来越流行。然而,大多数 GC 分析时间都很长。相比之下,超快速 GC 可以在几十秒内实现非常快速的分析,同时达到相当高的分辨率。反过来,将这种超快速 GC 与 IMS 耦合需要足够高的记录完整 IMS 光谱的重复率,以解析短的 GC 峰。因此,我们提出了一种重复率为 100 Hz 的漂移管 IMS。关键是有效检测器体积小,漂移长度短。因此,IMS 的离子源将小的反应区域与扩展的场切换离子快门和优化的气体流相结合。为了用半峰全宽为 100 ms 的最短 GC 峰解析完整的 IMS 光谱,仅使用了 41 mm 的短漂移长度,每个光谱的测量时间为 10 ms,因此在最短的 GC 峰上有十个数据点。为了避免样品冷凝,整个 IMS 被等温热至 120°C。尽管漂移时间短且温度高,IMS 仍能达到 60 的高分辨率。超快速 GC-IMS 达到了低 ppb 范围内的低检测限。为了演示,在 <30 s 内分析了酮混合物和三种不同的啤酒花品种。

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