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Updated: Aug 12, 2026

Gas Chromatography-Mass Spectrometry Paired with Total Vaporization Solid-Phase Microextraction as a Forensic Tool
Published on: May 25, 2021
Headspace solid-phase microextraction procedures for gas chromatographic analysis of biological fluids and materials
1School of Pharmacy and Biomedical Sciences, University of Portsmouth, UK. graham.mills@port.ac.uk
Headspace solid-phase microextraction (SPME) offers a solventless method for analyzing volatile and semivolatile compounds in biological samples. This review details its application in gas chromatography for diverse matrices like urine, blood, and breath.
Area of Science:
- Analytical Chemistry
- Biochemistry
Background:
- Solid-phase microextraction (SPME) is an emerging solventless technique for sample preparation.
- Headspace SPME coupled with gas chromatography (GC) is increasingly utilized for analyzing volatile and semivolatile compounds.
Purpose of the Study:
- To provide an updated review of headspace SPME applications in biological fluid and material analysis.
- To cover apparatus, fiber types, extraction conditions, and derivatization procedures.
- To discuss the analysis of various analytes including drugs, metabolites, solvents, pesticides, and endogenous compounds.
Main Methods:
- Review of existing literature on headspace SPME techniques.
- Focus on GC separation for volatile and semivolatile analyte extraction.
- Examination of diverse biological matrices: urine, blood, feces, breast milk, hair, breath, and saliva.
Main Results:
- Detailed overview of SPME methods for specific analytes within each biological matrix.
- Outlined experimental conditions and provided specific examples for various analyses.
- Highlighted the versatility of SPME across a wide range of biological samples and compound classes.
Conclusions:
- Headspace SPME is a valuable and widely adopted technique for biological sample analysis.
- Future potential includes new device development, advanced fiber chemistries, and coupling with high-performance liquid chromatography (HPLC).
- SPME offers a greener and more efficient alternative to traditional sample preparation methods.
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