title: Automated solid-phase extraction-liquid chromatography-tandem mass spectrometry analysis of 11-nor-Delta9-tetrahydrocannabinol-9-carboxylic acid in human urine specimens: application to a high-throughput urine analysis laboratory.
abstract: An automated solid-phase extraction coupled with liquid chromatography and tandem mass spectrometry (SPE-LC-MS-MS) method for the analysis of 11-nor-Delta(9)-tetrahydrocannabinol-9-carboxylic acid (THC-COOH) in human urine specimens was developed. The method was linear (R(2) = 0.9986) to 1000 ng/mL with no carryover evidenced at 2000 ng/mL. Limits of quantification and detection were found to be 2 ng/mL. Interrun precision was evaluated at the 15 ng/mL level over nine batches spanning 15 days (n = 45). The coefficient of variation (%CV) was found to be 5.5% over the course of the validation. Intrarun precision of a 15 ng/mL control (n = 5) ranged from 0.58% CV to 7.4% CV for the same set of analytical batches. Interference was tested using (+/-)-11-hydroxy-Delta(9)-tetrahydrocannabinol, cannabidiol, (-)-Delta(8)-tetrahydrocannabinol, and cannabinol. One hundred and nineteen specimens previously found to contain THC-COOH by a previously validated gas chromatographic mass spectrometry (GC-MS) procedure were compared to the SPE-LC-MS-MS method. Excellent agreement was found (R(2) = 0.9925) for the parallel comparison study. The automated SPE procedure eliminates the human factors of specimen handling, extraction, and derivatization, thereby reducing labor costs and rework resulting from human error or technique issues. Additionally, method runtime is greatly reduced (e.g., during parallel studies the SPE-LC-MS-MS instrument was often finished with analysis by the time the technician finished the offline SPE and derivatization procedure prior to the GC-MS analysis).
authors.affiliation: US Navy Drug Screening Laboratory, San Diego, California 92134-7040, USA.
authors.forename: P V
authors.initials: PV
authors.lastname: Robandt
authors.forename: K L
authors.initials: KL
authors.lastname: Klette
authors.forename: M
authors.initials: M
authors.lastname: Sibum
mesh_terms: D002851:Chromatography, High Pressure Liquid; D013759:Dronabinol / Q000031:analogs & derivatives* / Q000652:urine; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D057166:High-Throughput Screening Assays / Q000379:methods*; D006801:Humans; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D015813:Substance Abuse Detection / Q000379:methods*; D053719:Tandem Mass Spectrometry; D013997:Time Factors
chemical_list: C016780:11-nor-delta(9)-tetrahydrocannabinol-9-carboxylic acid; D013759:Dronabinol