Published: Journal of Analytical Toxicology, ISSN 0146-4760, Volume 25, Number 7, October, pp. 550-554

Solid-Phase Extraction and GC–MS Analysis of THC-COOH Method Optimized for a High-Throughput Forensic Drug-Testing Laboratory
Peter R. Stout, Carl K. Horn, and Kevin L. Klette
Navy Drug Screening Laboratory, P.O. Box 113, Bldg. H-2033, Naval Air Station, Jacksonville, Florida 32212

In order to facilitate the confirmation analysis of large numbers of urine samples previously screened positive for D⁹-tetrahydrocannabinol (THC), an extraction, derivitization, and GC–MS analysis method was developed. This method utilized a positive pressure manifold anion-exchange polymer-based solid-phase extraction followed by elution directly into the automated liquid sampling (ALS) vials. Rapid derivitization was accomplished using pentafluoropropionic anhydride/pentafluoropropanol (PFPA/PFPOH). Recoveries averaged 95% with a limit of detection of 0.875 ng/mL with a 3-mL sample volume. Performance of 11-nor-D⁹-tetrahydrocannabinol-9-carboxylic acid (THC-COOH)-d₃ and THC-COOH-d₉ internal standards were evaluated. The method was linear to 900 ng/mL THC-COOH using THC-COOH-d₉ with negligible contribution from the internal standard to very weak samples. Excellent agreement was seen with previous quantitations of human urine samples. More than 1000 human urine samples were analyzed using the method with 300 samples analyzed using an alternate qualifier ion (m/z 622) after some interference was observed with a qualifier ion (m/z 489). The 622 ion did not exhibit any interference even in samples with interfering peaks present in the 489 ion. The method resulted in dramatic reductions in processing time, waste production, and exposure hazards to laboratory personnel.

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