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Solution NMR Spectroscopy with Isotope-Labeled Cysteine (13C and 15N) Reveals the Surface Structure of l-Cysteine-Coated Ultrasmall Gold Nanoparticles (1.8 nm)
Langmuir ( IF 3.7 ) Pub Date : 2018-12-21 00:00:00 , DOI: 10.1021/acs.langmuir.8b03840 Tatjana Ruks , Christine Beuck , Torsten Schaller , Felix Niemeyer , Manfred Zähres , Kateryna Loza , Marc Heggen 1 , Ulrich Hagemann , Christian Mayer , Peter Bayer , Matthias Epple
Langmuir ( IF 3.7 ) Pub Date : 2018-12-21 00:00:00 , DOI: 10.1021/acs.langmuir.8b03840 Tatjana Ruks , Christine Beuck , Torsten Schaller , Felix Niemeyer , Manfred Zähres , Kateryna Loza , Marc Heggen 1 , Ulrich Hagemann , Christian Mayer , Peter Bayer , Matthias Epple
Affiliation
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Ultrasmall gold nanoparticles with a diameter of 1.8 nm were synthesized by reduction of tetrachloroauric acid with sodium borohydride in the presence of l-cysteine, with natural isotope abundance as well as 13C-labeled and 15N-labeled. The particle diameter was determined by high-resolution transmission electron microscopy and differential centrifugal sedimentation. X-ray photoelectron spectroscopy confirmed the presence of metallic gold with only a few percent of oxidized Au(+I) species. The surface structure and the coordination environment of the cysteine ligands on the ultrasmall gold nanoparticles were studied by a variety of homo- and heteronuclear NMR spectroscopic techniques including 1H–13C-heteronuclear single-quantum coherence and 13C–13C-INADEQUATE. Further information on the binding situation (including the absence of residual or detached l-cysteine in the solution) and on the nanoparticle diameter (indicating the well-dispersed state) was obtained by diffusion-ordered spectroscopy (1H-, 13C-, and 1H-13C-DOSY). Three coordination environments of l-cysteine on the gold surface were identified that were ascribed to different crystallographic sites, supported by geometric considerations of the nanoparticle ultrastructure. The particle size data and the NMR-spectroscopic analysis gave a particle composition of about Au174(cysteine)67.
中文翻译：
同位素标记的半胱氨酸（13 C和15 N）的溶液NMR光谱揭示了I-半胱氨酸涂层的超小金纳米颗粒（1.8 nm）的表面结构
通过在具有天然同位素丰度以及13 C标记和15 N标记的1-半胱氨酸存在下，用硼氢化钠将四氯金酸还原，可以合成出直径为1.8 nm的超小金纳米粒子。通过高分辨率透射电子显微镜和差速离心沉降法测定粒径。X射线光电子能谱证实了金属金的存在，其中只有百分之几的氧化的Au（+ I）物种。通过各种同核和异核NMR光谱技术，包括1 H– 13，研究了超小金纳米颗粒上半胱氨酸配体的表面结构和配位环境。C-异核单量子相干和13 C- 13 C-不足。对结合状况的进一步资料（包括没有残余的或分离的升通过扩散有序光谱（获得（指示良好分散的状态）在溶液中-半胱氨酸），并且在纳米颗粒直径1 H-，13 C-，和1 H - 13 C-DOSY）。l的三个协调环境鉴定出金表面上的-半胱氨酸归因于不同的晶体学位点，并由纳米颗粒超微结构的几何考虑所支持。粒度数据和NMR光谱分析给出约Au 174（半胱氨酸）67的颗粒组成。
更新日期：2018-12-21
中文翻译：
同位素标记的半胱氨酸（13 C和15 N）的溶液NMR光谱揭示了I-半胱氨酸涂层的超小金纳米颗粒（1.8 nm）的表面结构
通过在具有天然同位素丰度以及13 C标记和15 N标记的1-半胱氨酸存在下，用硼氢化钠将四氯金酸还原，可以合成出直径为1.8 nm的超小金纳米粒子。通过高分辨率透射电子显微镜和差速离心沉降法测定粒径。X射线光电子能谱证实了金属金的存在，其中只有百分之几的氧化的Au（+ I）物种。通过各种同核和异核NMR光谱技术，包括1 H– 13，研究了超小金纳米颗粒上半胱氨酸配体的表面结构和配位环境。C-异核单量子相干和13 C- 13 C-不足。对结合状况的进一步资料（包括没有残余的或分离的升通过扩散有序光谱（获得（指示良好分散的状态）在溶液中-半胱氨酸），并且在纳米颗粒直径1 H-，13 C-，和1 H - 13 C-DOSY）。l的三个协调环境鉴定出金表面上的-半胱氨酸归因于不同的晶体学位点，并由纳米颗粒超微结构的几何考虑所支持。粒度数据和NMR光谱分析给出约Au 174（半胱氨酸）67的颗粒组成。
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