Quantitative MALDI-TOF Mass Spectrometry of Star-Shaped Polylactides Based on Chromatographic Hyphenation.

IF 2.7 2区 化学 Q2 BIOCHEMICAL RESEARCH METHODS Journal of the American Society for Mass Spectrometry Pub Date : 2025-03-05 Epub Date: 2025-01-30 DOI:10.1021/jasms.4c00491
Jana Falkenhagen, Mete-Sungur Dalgic, Steffen M Weidner
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Abstract

The end groups of three- and four-arm star-shaped polylactides (PLA) with trimethylolpropane and pentaerythritol core structures were functionalized with acetic acid. Reaction products with different degrees of functionalization were analyzed by matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry. Additional gradient elution liquid adsorption chromatography (GELAC) measurements were performed to determine the degree of functionalization. This technique enabled clear separation and sufficient quantification of the formed species. These chromatographic data could be used inversely to quantify mass spectrometric results, which are usually biased by the unknown ionization probabilities of different polymer end group structures. Our results showed that, in this particular case, the peak intensity in the MALDI-TOF mass spectra can be used to semiquantitatively determine the degree of functionalization in incompletely functionalized multiarm PLA.

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基于色谱连字法的星形聚乳酸定量MALDI-TOF质谱分析。
以三甲基丙烷和季戊四醇为核心结构的三臂和四臂星形聚乳酸(PLA)的端基用乙酸进行了功能化。采用基质辅助激光解吸/电离飞行时间(MALDI-TOF)质谱法对不同功能化程度的反应产物进行了分析。另外进行梯度洗脱液相吸附色谱(GELAC)测量以确定功能化程度。该技术能够对形成的物种进行清晰的分离和充分的定量。这些色谱数据可以反向用于量化质谱分析结果,而质谱分析结果通常会受到不同聚合物端基结构的未知电离概率的影响。我们的研究结果表明,在这种特殊情况下,MALDI-TOF质谱中的峰强度可以半定量地确定不完全功能化多臂PLA的功能化程度。
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来源期刊
CiteScore
5.50
自引率
9.40%
发文量
257
审稿时长
1 months
期刊介绍: The Journal of the American Society for Mass Spectrometry presents research papers covering all aspects of mass spectrometry, incorporating coverage of fields of scientific inquiry in which mass spectrometry can play a role. Comprehensive in scope, the journal publishes papers on both fundamentals and applications of mass spectrometry. Fundamental subjects include instrumentation principles, design, and demonstration, structures and chemical properties of gas-phase ions, studies of thermodynamic properties, ion spectroscopy, chemical kinetics, mechanisms of ionization, theories of ion fragmentation, cluster ions, and potential energy surfaces. In addition to full papers, the journal offers Communications, Application Notes, and Accounts and Perspectives
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