大体积叔丁基硫醇连接金纳米粒子的离子迁移-串联质谱法。

IF 1.9 3区 化学 Q3 BIOCHEMICAL RESEARCH METHODS Journal of Mass Spectrometry Pub Date : 2024-01-24 DOI:10.1002/jms.4998
Kalpani H. Wijesinghe, Christopher Hood, Daniell Mattern, Laurence A. Angel, Amala Dass
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引用次数: 0

摘要

金纳米粒子(AuNPs)的合成范围为 1-3 纳米,具有特定数量的金核心原子和外层保护配体。由于其有趣的物理和化学特性,它们已成为近几十年来的 "热门话题 "之一。尽管有些 AuNPs 因未成功结晶而结构不明,但其结构的表征通常是通过晶体 X 射线衍射来实现的。研究 AuNPs 结构的另一种方法是电喷雾离子迁移串联质谱法(ESI-IMS-MSMS)。这项研究评估了使用市售的 Waters Synapt XS 仪器进行 ESI-IM-MSMS 分析如何有效地从两种 AuNPs(Au23 (S-tBu)16 和 Au30 (S-tBu)18)中获得有用的结构信息。该研究利用最大范围的碰撞能量和离子迁移率分离来测量产物离子的能量依赖性及其漂移时间,漂移时间是其空间尺寸的测量值。对于 Au23 (S-tBu)16,解离得到了外层保护单体 [RS-Au-SR] 和三聚体 [SR-Au-SR-Au-SR-Au-SR-Au-SR] 主链(其中 R = tBu)的质量,外层 Au 和 tBu 基团完全解离,显示出 Au15 S8 内核。对于 Au30 (S-tBu)18,解离产物主要是通过部分配体 S-tBu 和 tBu 从外层保护层中脱落以及单个 Au4 (S-tBu)4 单元的脱落。这些结果表明,对较小的 Au23 (S-tBu)16 进行 ESI-IM-MSMS 分析,可以获得其所有主要结构成分的信息,而对于 Au30 (S-tBu)18,整体结构信息仅限于外层配体。
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Ion mobility–tandem mass spectrometry of bulky tert-butyl thiol ligated gold nanoparticles

Gold nanoparticles (AuNPs) synthesized in the 1–3 nm range have a specific number of gold core atoms and outer protecting ligands. They have become one of the “hot topics” in recent decades because of their interesting physical and chemical properties. The characterization of their structures is usually achieved by crystal X-ray diffraction although the structures of some AuNPs remain unknown because they have not been successfully crystallized. An alternative method for studying the structure of AuNPs is electrospray ionization–ion mobility–tandem mass spectrometry (ESI-IM-MSMS). This research evaluated how effectively ESI-IM-MSMS using the commercially available Waters Synapt XS instrument yielded useful structural information from two AuNPs; Au23(S-tBu)16 and Au30(S-tBu)18. The study used the maximum range of available collision energies along with ion mobility separation to measure the energy-dependence of the product ions and their drift times which is a measure of their spatial size. For Au23(S-tBu)16, the dissociation gave the masses of the outer protecting monomeric [RS–Au–SR] and trimeric [SR–Au–SR–Au–SR–Au–SR] staples where R = tBu, and complete dissociation of the outer layer Au and tBu groups to reveal the Au15S8 core. For Au30(S-tBu)18, the dissociation products was primarily through the loss of the partial ligands S-tBu and tBu from the outer protecting layer and the loss of single Au4(S-tBu)4 unit. These results showed the that ESI-IM-MSMS analysis of the smaller Au23(S-tBu)16 gave information on all it major structural components whereas for Au30(S-tBu)18, the overall structural information was limited to the ligands of the outer layer.

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来源期刊
Journal of Mass Spectrometry
Journal of Mass Spectrometry 化学-光谱学
CiteScore
5.10
自引率
0.00%
发文量
84
审稿时长
1.5 months
期刊介绍: The Journal of Mass Spectrometry publishes papers on a broad range of topics of interest to scientists working in both fundamental and applied areas involving the study of gaseous ions. The aim of JMS is to serve the scientific community with information provided and arranged to help senior investigators to better stay abreast of new discoveries and studies in their own field, to make them aware of events and developments in associated fields, and to provide students and newcomers the basic tools with which to learn fundamental and applied aspects of mass spectrometry.
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