Substrate-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry of Some Small Biomolecules Using TiO2-Nanotubes: The Effect of Nanotube Diameter and Salt Addition

J Am Soc Mass Spectrom. 2023 Mar 1;34(3):374-382. doi: 10.1021/jasms.2c00246. Epub 2023 Jan 24.

Abstract

Substrate-assisted laser desorption/ionization (SALDI) is a kind of soft ionization method that is most suitable for the analysis of low molecular weight analytes when it is coupled with a time-of-flight mass spectrometer. Unlike the conventional matrix-assisted laser desorption/ionization, there is no interference in the SALDI with matrices for the low mass analyte peaks (m/z < 700). The focus of this work is to develop substrates based on nanomaterials to obtain higher sensitivity, better reproducibility, and easier preparation. The mass spectra of some small molecules (capecitabine, hemin, methadone, noscapine, oxycodone, thebaine, malathion, chlorpyrifos, ethion, permethrin, and phosalone) deposited on the TiO2-nanotube (TiO2-NTs) plate by the SALDI-TOF-MS technique are reported. The nanotubes are synthesized in different diameter sizes of nanotubes via the anodizing method. The intensity of the analyte peaks and the softness of ionization are optimized by varying the diameter of nanotubes and adding relevant alkali salts to the analytes. In addition, the reproducibility of the signal intensity of analytes is optimized by changing the surface hydrophilicity of the TiO2-NT plate.

Keywords: SALDI-TOF-MS; TiO2−nanotube; laser mass spectrometry; low molecular weight compounds; nanomaterial.