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Updated: Jan 13, 2026

Synthesis and Characterization of Amphiphilic Gold Nanoparticles
Published on: July 2, 2019
Unravelling the speciation of gold(I) fluorinated benzenethiolates using hyphenated HPLC/ICP-AES and HPLC/ESI-MS
Victoria V Volchek1, Dmitriy G Sheven1, Pavel A Tkachenko1
1Nikolaev Institute of Inorganic Chemistry SB RAS, 3 Acad. Lavrentiev Ave., Novosibirsk, 630090, Russia.
Abstract:
Gold(I) fluorinated benzenethiolates, H[Au(SR)2] R = C6F5, C6F4H, C6F4CF3, C6F4Cl), are widely believed as the precursors in catalysis and nanomaterials science, but their speciation remains complex due to the dynamic equilibria. Unravelling these species is essential for understanding their reactivity and applications. This study employs hyphenated high-performance liquid chromatography (HPLC) coupled with inductively coupled plasma atomic emission spectrometry (ICP-AES) and electrospray ionization mass spectrometry (ESI-MS), combining preliminary separation with subsequent online elemental and molecular characterization for comprehensive identification of the coexisting species in complex solutions. Chromatographic separation resolved three peaks for each gold complex assigned as disulfide (RSSR) and gold species: H[AuI(SR)2] and H[AuIII(SR)4], UV-vis spectra of the eluted peaks further confirmed the assignment. The stoichiometric Au:S ratios of 1:2 and 1:4 for the second and third peaks were measured by HPLC/ICP-AES, while HPLC/ESI-MS data confirmed the presence of the gold(I) fluorinated benzenethiolates [Au(SR)2]- and unambiguously identified the gold(III) species [Au(SR)4]-. These results facilitate the development of stable gold-thiolate complexes for catalytic and materials science applications, while demonstrating the power of hyphenated analytical techniques for speciation studies in inorganic and organometallic chemistry.
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