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Updated: Jan 26, 2026

Gas Chromatography-Mass Spectrometry Paired with Total Vaporization Solid-Phase Microextraction as a Forensic Tool
Published on: May 25, 2021
In-situ derivatization and headspace solid-phase microextraction for gas chromatography-mass spectrometry analysis of
Hyunsuk Kim1, Yungyeong Cho2, Bong Soo Lee3
1Center for Cell-Encapsulation Research, Department of Chemistry, KAIST, Daejeon, 34141, South Korea; Chemical and Biological Defense Department, Agency for Defense Development, Daejeon, 34186, South Korea.
Abstract:
A headspace solid-phase microextraction (HS-SPME) method, involving solid-phase extraction and in-situ derivatization using polymeric thin film, was developed for the gas chromatography-mass spectrometry (GC-MS) analysis of the degradation products of nerve agents. The solid-phase extraction (SPE) was performed using poly([2-(Methacryloyloxy)ethyl]trimethylammonium chloride) film on a gold plate prepared via surface-initiated polymerization. The extracted analytes were directly derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) on the plate. Various parameters like fiber type, headspace time, temperature, and amount of BSTFA were optimized. Under the optimized conditions, the relative standard deviations (RSDs) were in the range 7.0-13.1% and the limits of detection (LODs) were measured to be between 10 and 20 pg mL-1. The application of the developed method was tested using the 35th Organization for Prohibition of Chemical Weapons (OPCW) proficiency test sample.
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