超临界流体色谱-串联质谱联用转移离子源中化学反应软电离的表征

IF 2.8 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Journal of separation science Pub Date : 2024-09-25 DOI:10.1002/jssc.202400500
Niray Bhakta, Alexander S. Kaplitz, Destini Black, Kevin A. Schug
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引用次数: 0

摘要

使用超临界流体色谱-质谱法(SFC-MS)对市售的介质阻挡放电离子源(DBDI)进行了测试。所研究的化合物混合物包括稀释在甲醇中的咖啡因、可可碱、茶碱、尿嘧啶、睾酮和芘。对不同浓度下的多次进样进行了动态响应范围评估。精密度研究表明,离子源在 10-1000 纳克/毫升的浓度范围内具有稳健性和灵敏度。实验结果表明,除可可碱的相对标准偏差(RSD)小于 10%(低至 25 纳克/毫升)外,所有受测分析物在该范围内的线性回归系数均大于或等于 0.99。值得注意的是,本研究首次调查了商用 DBDI 源与 SFC 耦合的灵敏度;所有化合物的检测限均小于 1 纳克/毫升。本研究证明了 SFC 色谱分离和 MS 分析可用于多环芳烃等传统常压电离效果不佳的化合物。将 SFC 与 DBDI 源相结合,为分析以前用标准大气压电离技术难以表征的化合物开辟了一条前景广阔的途径。
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Characterization of a Soft Ionization by Chemical Reaction in Transfer Ion Source Hyphenated With Supercritical Fluid Chromatography-Tandem Mass Spectrometry

A commercially available dielectric barrier discharge ionization (DBDI) source was tested with supercritical fluid chromatography-mass spectrometry (SFC-MS). The compound mixture investigated comprised caffeine, theobromine, theophylline, uracil, testosterone, and pyrene, diluted in methanol. Dynamic response ranges were evaluated with multiple injections at different concentrations. Precision studies demonstrated the robustness and sensitivity of the ionization source across a concentration range of 10–1000 ng/mL. Results from this experiment showed linear regression of 0.99 or greater for all analytes tested over the range with a relative standard deviation (RSD) of less than 10% down to 10 ng/mL for all analytes except theobromine, which had an RSD of less than 10% down to 25 ng/mL. Notably, this study marks the first investigation of sensitivity for coupling a commercial DBDI source with SFC; a limit of detection less than 1 ng/mL was achieved for all compounds. This study demonstrates chromatographic separation by SFC and MS analysis for compounds that ionize poorly using traditional atmospheric pressure ionization, such as polycyclic aromatic hydrocarbons. Combining SFC with the DBDI source opens promising avenues for analyzing compounds that were previously challenging to characterize with standard atmospheric pressure ionization techniques.

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来源期刊
Journal of separation science
Journal of separation science 化学-分析化学
CiteScore
6.30
自引率
16.10%
发文量
408
审稿时长
1.8 months
期刊介绍: The Journal of Separation Science (JSS) is the most comprehensive source in separation science, since it covers all areas of chromatographic and electrophoretic separation methods in theory and practice, both in the analytical and in the preparative mode, solid phase extraction, sample preparation, and related techniques. Manuscripts on methodological or instrumental developments, including detection aspects, in particular mass spectrometry, as well as on innovative applications will also be published. Manuscripts on hyphenation, automation, and miniaturization are particularly welcome. Pre- and post-separation facets of a total analysis may be covered as well as the underlying logic of the development or application of a method.
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