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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
Headspace gas chromatography for the determination of volatile methylsiloxanes in personal care products
Juan Aspromonte1, Giulia Giacoppo1,2, Kris Wolfs1
1Department of Pharmaceutical and Pharmacological Sciences, Pharmaceutical Analysis, KU Leuven - University of Leuven, Herestraat 49, O&N2, PB 923, 3000, Leuven, Belgium.
Abstract:
Most of the reported methods for the analysis of volatile methylsiloxanes focus on their environmental fate or possible health effects, aiming at trace level analysis by using direct injection gas chromatography. However, system contamination as carry over and side reactions at the injector are commonly reported in those cases. In this article, we explore the use of headspace gas chromatography combined with the total vaporization technique as an alternative to avoid such issues for the analysis of linear (L2-L5) and cyclic (D3-D5) volatile methylsiloxanes. The proposed method showed good linearity with R2 values higher than 0.9961 and no significant contribution (α = 0.05) of the intercept. The limit of detection was always below 0.11 μg/vial (0.0025% m/m). Finally, the method was applied to real samples like an adhesive remover, hair oil, shampoo, and cream. After simple sample pretreatment, recoveries higher than 86% were achieved. Graphical abstract.
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