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A semi-automated solid-phase extraction liquid chromatography/tandem mass spectrometry method for the analysis of tetrahydrocannabinol and metabolites in whole blood.

Abstract

Marijuana is one of the most commonly abused illicit substances in the USA, making cannabinoids important to detect in clinical and forensic toxicology laboratories. Historically, cannabinoids in biological fluids have been derivatized and analyzed by gas chromatography/mass spectrometry (GC/MS). There has been a gradual shift in many laboratories towards liquid chromatography/mass spectrometry (LC/MS) for this analysis due to its improved sensitivity and reduced sample preparation compared with GC/MS procedures. This paper reports a validated method for the analysis of Delta(9)-tetrahydrocannabinol (THC) and its two main metabolites, 11-nor-9-carboxy-Delta(9)-tetrahydrocannabinol (THC-COOH) and 11-hydroxy-Delta(9)-tetrahydrocannabinol (THC-OH), in whole blood samples. The method has also been validated for cannabinol (CBD) and cannabidiol (CDN), two cannabinoids that were shown not to interfere with the method. This method has been successfully applied to samples both from living people and from deceased individuals obtained during autopsy. This method utilizes online solid-phase extraction (SPE) with LC/MS. Pretreatment of samples involves protein precipitation, sample concentration, ultracentrifugation, and reconstitution. The online SPE procedure was developed using Hysphere C8-EC sorbent. A chromatographic gradient with an Xterra MS C(18) column was used for the separation. Four multiple-reaction monitoring (MRM) transitions were monitored for each analyte and internal standard. Linearity generally fell between 2 and 200 ng/mL. The limits of detection (LODs) ranged from 0.5 to 3 ng/mL and the limits of quantitation (LOQs) ranged from 2 to 8 ng/mL. The bias and imprecision were determined using a simple analysis of variance (ANOVA: single factor). The results demonstrate bias as <7%, and imprecision as <9%, for all components at each quantity control level.

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  • Publisher Full Text
  • Authors+Show Affiliations

    ,

    Federal Bureau of Investigation Laboratory, Quantico, VA 22135, USA. Eshwar.Jagerdeo@ic.fbi.gov

    , ,

    Source

    MeSH

    Chromatography, Liquid
    Dronabinol
    Humans
    Solid Phase Extraction
    Tandem Mass Spectrometry

    Pub Type(s)

    Evaluation Studies
    Journal Article

    Language

    eng

    PubMed ID

    19630026

    Citation

    TY - JOUR T1 - A semi-automated solid-phase extraction liquid chromatography/tandem mass spectrometry method for the analysis of tetrahydrocannabinol and metabolites in whole blood. AU - Jagerdeo,Eshwar, AU - Schaff,Jason E, AU - Montgomery,Madeline A, AU - LeBeau,Marc A, PY - 2009/7/25/entrez PY - 2009/7/25/pubmed PY - 2009/10/8/medline SP - 2697 EP - 705 JF - Rapid communications in mass spectrometry : RCM JO - Rapid Commun. Mass Spectrom. VL - 23 IS - 17 N2 - Marijuana is one of the most commonly abused illicit substances in the USA, making cannabinoids important to detect in clinical and forensic toxicology laboratories. Historically, cannabinoids in biological fluids have been derivatized and analyzed by gas chromatography/mass spectrometry (GC/MS). There has been a gradual shift in many laboratories towards liquid chromatography/mass spectrometry (LC/MS) for this analysis due to its improved sensitivity and reduced sample preparation compared with GC/MS procedures. This paper reports a validated method for the analysis of Delta(9)-tetrahydrocannabinol (THC) and its two main metabolites, 11-nor-9-carboxy-Delta(9)-tetrahydrocannabinol (THC-COOH) and 11-hydroxy-Delta(9)-tetrahydrocannabinol (THC-OH), in whole blood samples. The method has also been validated for cannabinol (CBD) and cannabidiol (CDN), two cannabinoids that were shown not to interfere with the method. This method has been successfully applied to samples both from living people and from deceased individuals obtained during autopsy. This method utilizes online solid-phase extraction (SPE) with LC/MS. Pretreatment of samples involves protein precipitation, sample concentration, ultracentrifugation, and reconstitution. The online SPE procedure was developed using Hysphere C8-EC sorbent. A chromatographic gradient with an Xterra MS C(18) column was used for the separation. Four multiple-reaction monitoring (MRM) transitions were monitored for each analyte and internal standard. Linearity generally fell between 2 and 200 ng/mL. The limits of detection (LODs) ranged from 0.5 to 3 ng/mL and the limits of quantitation (LOQs) ranged from 2 to 8 ng/mL. The bias and imprecision were determined using a simple analysis of variance (ANOVA: single factor). The results demonstrate bias as <7%, and imprecision as <9%, for all components at each quantity control level. SN - 1097-0231 UR - https://www.unboundmedicine.com/medline/citation/19630026/abstract/A_semi_automated_solid_phase_extraction_liquid_chromatography/tandem_mass_spectrometry_method_for_the_analysis_of_tetrahydrocannabinol_and_metabolites_in_whole_blood_ L2 - https://doi.org/10.1002/rcm.4174 ER -