Preprint Article Version 1 Preserved in Portico This version is not peer-reviewed

Efficient Analysis of Small Molecules via Laser Desorption/Ionization Time-of-Flight Mass Spectrometry (LDI–TOF MS) Using Gold Nanoshells with Nanogaps

Version 1 : Received: 22 August 2023 / Approved: 23 August 2023 / Online: 24 August 2023 (03:40:39 CEST)

How to cite: Kim, N.; Kim, Y.; Yoo, J.; Park, S.; Jun, B.; Yeo, W. Efficient Analysis of Small Molecules via Laser Desorption/Ionization Time-of-Flight Mass Spectrometry (LDI–TOF MS) Using Gold Nanoshells with Nanogaps. Preprints 2023, 2023081675. https://doi.org/10.20944/preprints202308.1675.v1 Kim, N.; Kim, Y.; Yoo, J.; Park, S.; Jun, B.; Yeo, W. Efficient Analysis of Small Molecules via Laser Desorption/Ionization Time-of-Flight Mass Spectrometry (LDI–TOF MS) Using Gold Nanoshells with Nanogaps. Preprints 2023, 2023081675. https://doi.org/10.20944/preprints202308.1675.v1

Abstract

Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI–TOF MS) is a commonly used technique for analyzing large biomolecules. However, the utilization of organic matrices limits the small-molecule analysis because of the interferences in the low-mass region and reproducibility issues. To overcome these limitations, a surface-assisted laser desorption/ionization (SALDI), which utilizes nanostructured metallic surfaces, has been developed. Herein, a novel approach for SALDI–MS was proposed using nanoengineered gold shell with nanogaps on the silica core (SiO2@Au NGS), which is an emerging material due to its excellent heat-generating capabilities. The gold shell thickness was controlled by adjusting the concentration of gold precursor for the growth of gold nanoparticles. SALDI-MS measurements were performed on a layer formed by drop-casting a mixture of SiO2@Au NGS and analytes. At the optimized process, the gold shell thickness was observed to be 17.2 nm, which showed the highest absorbance. The ion desorption efficiency was confirmed with a survival yield upon fragmentation. Based on the enhanced SALDI capability, SiO2@Au NGS was utilized to detect various small molecules including amino acids, sugars, and flavonoids. The limits of detection, reproducibility, and salt tolerance of SiO2@Au NGS demonstrate its potential as an effective and reliable SALDI material for small-molecule analyses.

Keywords

Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry; gold nanoshell; nanogap; surface-assisted laser desorption/ionization; silica core nanoparticle; small-molecule analysis

Subject

Chemistry and Materials Science, Analytical Chemistry

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