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Validated method for the simultaneous determination of Delta9-THC and Delta9-THC-COOH in oral fluid, urine and whole blood using solid-phase extraction and liquid chromatography-mass spectrometry with electrospray ionization.
Forensic Sci Int. 2007 Aug 06; 170(2-3):148-55.FS

Abstract

A fully validated, sensitive and specific method for the extraction and quantification of Delta(9)-tetrahydrocannabinol (THC) and 11-nor-9-carboxy-Delta(9)-THC (THC-COOH) and for the detection of 11-hydroxy-Delta(9)-THC (11-OH THC) in oral fluid, urine and whole blood is presented. Solid-phase extraction and liquid chromatography-mass spectrometry (LC-MS) technique were used, with electrospray ionization. Three ions were monitored for THC and THC-COOH and two for 11-OH THC. The compounds were quantified by selected ion recording of m/z 315.31, 329.18 and 343.16 for THC, 11-OH THC and THC-COOH, respectively, and m/z 318.27 and 346.26 for the deuterated internal standards, THC-d(3) and THC-COOH-d(3), respectively. The method proved to be precise for THC and THC-COOH both in terms of intra-day and inter-day analysis, with intra-day coefficients of variation (CV) less than 6.3, 6.6 and 6.5% for THC in saliva, urine and blood, respectively, and 6.8 and 7.7% for THC-COOH in urine and blood, respectively. Day-to-day CVs were less than 3.5, 4.9 and 11.3% for THC in saliva, urine and blood, respectively, and 6.2 and 6.4% for THC-COOH in urine and blood, respectively. Limits of detection (LOD) were 2 ng/mL for THC in oral fluid and 0.5 ng/mL for THC and THC-COOH and 20 ng/mL for 11-OH THC, in urine and blood. Calibration curves showed a linear relationship for THC and THC-COOH in all samples (r(2)>0.999) within the range investigated. The procedure presented here has high specificity, selectivity and sensitivity. It can be regarded as an alternative method to GC-MS for the confirmation of positive immunoassay test results, and can be used as a suitable analytical tool for the quantification of THC and THC-COOH in oral fluid, urine and/or blood samples.

Authors+Show Affiliations

Delegation of Coimbra, National Institute of Legal Medicine, Coimbra, Portugal. helenateixeira@dcinml.mj.ptNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Validation Study

Language

eng

PubMed ID

17614225

Citation

Teixeira, Helena, et al. "Validated Method for the Simultaneous Determination of Delta9-THC and Delta9-THC-COOH in Oral Fluid, Urine and Whole Blood Using Solid-phase Extraction and Liquid Chromatography-mass Spectrometry With Electrospray Ionization." Forensic Science International, vol. 170, no. 2-3, 2007, pp. 148-55.
Teixeira H, Verstraete A, Proença P, et al. Validated method for the simultaneous determination of Delta9-THC and Delta9-THC-COOH in oral fluid, urine and whole blood using solid-phase extraction and liquid chromatography-mass spectrometry with electrospray ionization. Forensic Sci Int. 2007;170(2-3):148-55.
Teixeira, H., Verstraete, A., Proença, P., Corte-Real, F., Monsanto, P., & Vieira, D. N. (2007). Validated method for the simultaneous determination of Delta9-THC and Delta9-THC-COOH in oral fluid, urine and whole blood using solid-phase extraction and liquid chromatography-mass spectrometry with electrospray ionization. Forensic Science International, 170(2-3), 148-55.
Teixeira H, et al. Validated Method for the Simultaneous Determination of Delta9-THC and Delta9-THC-COOH in Oral Fluid, Urine and Whole Blood Using Solid-phase Extraction and Liquid Chromatography-mass Spectrometry With Electrospray Ionization. Forensic Sci Int. 2007 Aug 6;170(2-3):148-55. PubMed PMID: 17614225.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Validated method for the simultaneous determination of Delta9-THC and Delta9-THC-COOH in oral fluid, urine and whole blood using solid-phase extraction and liquid chromatography-mass spectrometry with electrospray ionization. AU - Teixeira,Helena, AU - Verstraete,Alain, AU - Proença,Paula, AU - Corte-Real,Francisco, AU - Monsanto,Paula, AU - Vieira,Duarte Nuno, Y1 - 2007/07/05/ PY - 2006/10/09/received PY - 2007/03/23/revised PY - 2007/03/23/accepted PY - 2007/7/7/pubmed PY - 2007/10/19/medline PY - 2007/7/7/entrez SP - 148 EP - 55 JF - Forensic science international JO - Forensic Sci Int VL - 170 IS - 2-3 N2 - A fully validated, sensitive and specific method for the extraction and quantification of Delta(9)-tetrahydrocannabinol (THC) and 11-nor-9-carboxy-Delta(9)-THC (THC-COOH) and for the detection of 11-hydroxy-Delta(9)-THC (11-OH THC) in oral fluid, urine and whole blood is presented. Solid-phase extraction and liquid chromatography-mass spectrometry (LC-MS) technique were used, with electrospray ionization. Three ions were monitored for THC and THC-COOH and two for 11-OH THC. The compounds were quantified by selected ion recording of m/z 315.31, 329.18 and 343.16 for THC, 11-OH THC and THC-COOH, respectively, and m/z 318.27 and 346.26 for the deuterated internal standards, THC-d(3) and THC-COOH-d(3), respectively. The method proved to be precise for THC and THC-COOH both in terms of intra-day and inter-day analysis, with intra-day coefficients of variation (CV) less than 6.3, 6.6 and 6.5% for THC in saliva, urine and blood, respectively, and 6.8 and 7.7% for THC-COOH in urine and blood, respectively. Day-to-day CVs were less than 3.5, 4.9 and 11.3% for THC in saliva, urine and blood, respectively, and 6.2 and 6.4% for THC-COOH in urine and blood, respectively. Limits of detection (LOD) were 2 ng/mL for THC in oral fluid and 0.5 ng/mL for THC and THC-COOH and 20 ng/mL for 11-OH THC, in urine and blood. Calibration curves showed a linear relationship for THC and THC-COOH in all samples (r(2)>0.999) within the range investigated. The procedure presented here has high specificity, selectivity and sensitivity. It can be regarded as an alternative method to GC-MS for the confirmation of positive immunoassay test results, and can be used as a suitable analytical tool for the quantification of THC and THC-COOH in oral fluid, urine and/or blood samples. SN - 1872-6283 UR - https://www.unboundmedicine.com/medline/citation/17614225/Validated_method_for_the_simultaneous_determination_of_Delta9_THC_and_Delta9_THC_COOH_in_oral_fluid_urine_and_whole_blood_using_solid_phase_extraction_and_liquid_chromatography_mass_spectrometry_with_electrospray_ionization_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0379-0738(07)00560-9 DB - PRIME DP - Unbound Medicine ER -