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Updated: Dec 28, 2025

Gas Chromatography-Mass Spectrometry Paired with Total Vaporization Solid-Phase Microextraction as a Forensic Tool
Published on: May 25, 2021
High-performance thin-layer chromatography with atmospheric solids analysis probe mass spectrometry for analysis of
Mathieu Beaumesnil1,2, Anna Luiza Mendes Siqueira1,2, Marie Hubert-Roux1
1Normandie Univ, COBRA, UMR6014 and FR3038, Université de Rouen, INSA de Rouen, CNRS, IRCOF, 1 rue Tesnière, 76821, Mont-Saint-Aignan Cedex, France.
Rationale:
The offline coupling of high-performance thin-layer chromatography (HPTLC) with atmospheric solids analysis probe mass spectrometry (ASAP-MS) was evaluated for the characterization of polymeric additives in gasoline.
Methods:
A protocol was developed to optimize the ion signal. A glass capillary was moistened with deionized water, and then dipped into silica gel scratched from an HPTLC plate. The capillary tube was fixed to the ASAP holder and introduced into the ionization source for analysis by MS. Silica gel, reversed-phase C18 and cellulose stationary phases were evaluated.
Results:
The effect of the stationary phase and the nature of analyte were evaluated using polypropylene glycol and polyisobutylene succinimide polyamine as analyte molecules. The optimal ionization conditions are significantly different between ASAP and HPTLC/ASAP-MS analyses. In particular, a higher desorption gas temperature was required to produce ions from the silica gel HPTLC plate. The presence of the stationary phase reduces the internal energy of the ions and limits the fragmentation.
Conclusions:
HPTLC/ASAP-MS is a very fast and efficient technique for the analysis of polymers in formulated fuels. Good ionization efficiency was obtained with all investigated stationary phases.
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