Forensic sample analysis using supercritical fluid extraction coupled with solid phase microextraction.

  • Emma-Jane Lee

    Student thesis: Doctoral Thesis


    A third of adults in the UK admit to using controlled substances at least once hi their lives and the most commonly abused drug was found to be cannabis, followed by the opiates and ecognine derivatives. Forensic laboratories are continually trying to reduce the turnaround time for samples submitted for analysis, to less than the current time of four days. One of the main aims of this work was to reduce the time taken to prepare, extract and analyse hair for target analytes. A new method combining supercritical fluid extraction and solid phase micro-extraction (SFE/SPME) is introduced.

    This coupled procedure utilises the advantages of using supercritical carbon dioxide as an extraction solvent and collecting the extract on a selected SPME fibre. Together the combined techniques provide a method that is solvent-free and highly selective, whilst reducing sample preparation to a minimum. Digested hair samples are examined by SEM to find the best method. Alkali hydrolysis and enzyme digestion using proteinase K were found to be the most effective pre-extraction methods. Solid hair samples with the addition of a derivatization reagent (BSTFA) gave the best results using the coupled technique. After optimisation and validation, the extraction from both real and spiked samples resulted in recoveries between 60% to 80% for the target analytes A9 -tetrahydrocannabinol (A9- THC) , cannabinol (CBN) and cannabidiol (CBD).

    Other forensic applications such as the extraction of polycyclic aromatic hydrocarbons and pesticides from environmental and food samples and the examination of fire debris for the presence of accelerants are also carried out. PAH could easily be extracted from complex matrices to give recoveries of up to 97% for some analytes at the optimized conditions of 90°C at 4500 psi over a 10 minute dynamic extraction period. Pesticide extraction gave recoveries of 60 - 80% while the extraction of accelerants from fire debris clearly showed that accelerants such as diesel can be identified over the coincidental PAH and hydrocarbon peaks found in burnt debris.

    The coupling of SFE to SPME provides an exciting technique that has a wide range of applications and creates potential for a fully automated on-line system.
    Date of AwardMar 2007
    Original languageEnglish
    SupervisorTony (Antony) Berry (Supervisor) & Alan Guwy (Supervisor)


    • Supercritical fluid extraction
    • Chemistry, Analytic
    • Technique

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