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On-line solid-phase extraction combined with liquid chromatography-tandem mass spectrometry for high throughput analysis of 11-nor-Delta9-tetrahydrocannabinol-9-carboxylic acid in urine.
J Chromatogr B Analyt Technol Biomed Life Sci. 2009 Jul 15; 877(22):2153-7.JC

Abstract

A simple, rapid and highly sensitive method for the analysis of THC-COOH in urine, using automated on-line solid-phase extraction (SPE) combined with liquid chromatography (LC)-mass spectrometry (MS/MS), is developed and fully validated according to international guidelines. Chromatographic separation was achieved on an Atlantis dC(18) column with an isocratical gradient, ensuring the elution of THC-COOH within 4.1 min. The total process time was 6 min and 500 microL of sample was required. SPE using C(8) cartridges was highly effective, reproducible and led to significant decreases in the interferences present in the matrix. The method showed an excellent intra- and inter-assay precision (relative standard deviation (RSD) <7% and bias <13%) for four external quality control (QC) samples and three 'in house' QCs. Responses were linear over the investigated range (r(2)>0.99, 5-200 microg/L). Limits of quantification (LOQ) and detection (LOD) were determined to be 5 micro/L and 0.25 microg/L, respectively. Furthermore, the analyte and the processed samples were demonstrated to be stable. Moreover, no carryover was observed after the analysis of high concentrated urine samples (5000 microg/L THC-COOH)). The method was subsequently applied to authentic samples previously screened by a routine immunoassay method.

Authors+Show Affiliations

Federal Public Service Justice, National Institute of Criminalistics and Criminology, Chaussee de Vilvorde 100, 1120 Brussels, Belgium. mariadelmar.ramirezfernandez@just.fgov.beNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Evaluation Study
Journal Article

Language

eng

PubMed ID

19535306

Citation

Fernández, María del Mar Ramírez, et al. "On-line Solid-phase Extraction Combined With Liquid Chromatography-tandem Mass Spectrometry for High Throughput Analysis of 11-nor-Delta9-tetrahydrocannabinol-9-carboxylic Acid in Urine." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 877, no. 22, 2009, pp. 2153-7.
Fernández Mdel M, Wille SM, Samyn N, et al. On-line solid-phase extraction combined with liquid chromatography-tandem mass spectrometry for high throughput analysis of 11-nor-Delta9-tetrahydrocannabinol-9-carboxylic acid in urine. J Chromatogr B Analyt Technol Biomed Life Sci. 2009;877(22):2153-7.
Fernández, M. d. e. l. . M., Wille, S. M., Samyn, N., Wood, M., López-Rivadulla, M., & De Boeck, G. (2009). On-line solid-phase extraction combined with liquid chromatography-tandem mass spectrometry for high throughput analysis of 11-nor-Delta9-tetrahydrocannabinol-9-carboxylic acid in urine. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 877(22), 2153-7. https://doi.org/10.1016/j.jchromb.2009.04.047
Fernández Mdel M, et al. On-line Solid-phase Extraction Combined With Liquid Chromatography-tandem Mass Spectrometry for High Throughput Analysis of 11-nor-Delta9-tetrahydrocannabinol-9-carboxylic Acid in Urine. J Chromatogr B Analyt Technol Biomed Life Sci. 2009 Jul 15;877(22):2153-7. PubMed PMID: 19535306.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - On-line solid-phase extraction combined with liquid chromatography-tandem mass spectrometry for high throughput analysis of 11-nor-Delta9-tetrahydrocannabinol-9-carboxylic acid in urine. AU - Fernández,María del Mar Ramírez, AU - Wille,Sarah M R, AU - Samyn,Nele, AU - Wood,Michelle, AU - López-Rivadulla,Manuel, AU - De Boeck,Gert, Y1 - 2009/05/21/ PY - 2008/12/18/received PY - 2009/04/20/revised PY - 2009/04/23/accepted PY - 2009/6/19/entrez PY - 2009/6/19/pubmed PY - 2009/10/9/medline SP - 2153 EP - 7 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 877 IS - 22 N2 - A simple, rapid and highly sensitive method for the analysis of THC-COOH in urine, using automated on-line solid-phase extraction (SPE) combined with liquid chromatography (LC)-mass spectrometry (MS/MS), is developed and fully validated according to international guidelines. Chromatographic separation was achieved on an Atlantis dC(18) column with an isocratical gradient, ensuring the elution of THC-COOH within 4.1 min. The total process time was 6 min and 500 microL of sample was required. SPE using C(8) cartridges was highly effective, reproducible and led to significant decreases in the interferences present in the matrix. The method showed an excellent intra- and inter-assay precision (relative standard deviation (RSD) <7% and bias <13%) for four external quality control (QC) samples and three 'in house' QCs. Responses were linear over the investigated range (r(2)>0.99, 5-200 microg/L). Limits of quantification (LOQ) and detection (LOD) were determined to be 5 micro/L and 0.25 microg/L, respectively. Furthermore, the analyte and the processed samples were demonstrated to be stable. Moreover, no carryover was observed after the analysis of high concentrated urine samples (5000 microg/L THC-COOH)). The method was subsequently applied to authentic samples previously screened by a routine immunoassay method. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/19535306/On_line_solid_phase_extraction_combined_with_liquid_chromatography_tandem_mass_spectrometry_for_high_throughput_analysis_of_11_nor_Delta9_tetrahydrocannabinol_9_carboxylic_acid_in_urine_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(09)00304-3 DB - PRIME DP - Unbound Medicine ER -