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This chapter provides a comprehensive comparative overview of extraction techniques utilized in forensic doping control for the identification of various classes of prohibited substances across biological matrices, including urine, plasma, and hair. Emphasis is placed on optimizing sample preparation to enhance analytical precision and reliability in both LC–MS and GC–MS analyses. Depending on the physicochemical properties of the target analytes, solid-phase extraction (SPE) and liquid–liquid extraction (LLE) were employed. Antihistamines, NSAIDs, corticosteroids, and anabolic steroids demonstrated efficient extraction through SPE in urine and LLE in plasma samples. Peptide-based drugs, myo-inositol trispyrophosphate (ITPP), and bisphosphonates achieved optimal recovery using SPE for both matrices, while quaternary ammonium compounds were effectively processed via direct dilution and injection (D&I). Furthermore, specialized protocols for hair extraction are presented, emphasizing their role in assessing long-term drug exposure. The chapter also explores the extraction and derivatization of non-polar and poorly ionizable compounds, such as specific anabolic steroids, which require chemical modification into volatile derivatives to enable GC–MS detection. In addition, the discussion extends to essential validation parameters such as selectivity, sensitivity, linearity, accuracy, precision, recovery, and matrix effects evaluated according to internationally recognized standards, including SWGTOX, ISO/IEC 17,025, and WADA guidelines. Overall, this comparative analysis underscores the significance of matrix-specific extraction and validation strategies in achieving robust, reproducible, and legally defensible results in forensic doping investigations.

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Comparative Case Studies on Extraction Methods for LC–MS and GC–MS Detection in Forensic Doping Control

  • 章节

  • 发表日期：

    2026年

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  • Abdul Khader Karakka Kal,
  • Michael Benedict Subhahar,
  • Tajudheen K. Karatt

摘要

This chapter provides a comprehensive comparative overview of extraction techniques utilized in forensic doping control for the identification of various classes of prohibited substances across biological matrices, including urine, plasma, and hair. Emphasis is placed on optimizing sample preparation to enhance analytical precision and reliability in both LC–MS and GC–MS analyses. Depending on the physicochemical properties of the target analytes, solid-phase extraction (SPE) and liquid–liquid extraction (LLE) were employed. Antihistamines, NSAIDs, corticosteroids, and anabolic steroids demonstrated efficient extraction through SPE in urine and LLE in plasma samples. Peptide-based drugs, myo-inositol trispyrophosphate (ITPP), and bisphosphonates achieved optimal recovery using SPE for both matrices, while quaternary ammonium compounds were effectively processed via direct dilution and injection (D&I). Furthermore, specialized protocols for hair extraction are presented, emphasizing their role in assessing long-term drug exposure. The chapter also explores the extraction and derivatization of non-polar and poorly ionizable compounds, such as specific anabolic steroids, which require chemical modification into volatile derivatives to enable GC–MS detection. In addition, the discussion extends to essential validation parameters such as selectivity, sensitivity, linearity, accuracy, precision, recovery, and matrix effects evaluated according to internationally recognized standards, including SWGTOX, ISO/IEC 17,025, and WADA guidelines. Overall, this comparative analysis underscores the significance of matrix-specific extraction and validation strategies in achieving robust, reproducible, and legally defensible results in forensic doping investigations.