A method was developed for quantitating 9-carboxy-ll-nor-A'-tetrahydrocannabinol in human urine as part of the process for validating an automated enzyme immunoassay for marijuana metabolites. Sample cleanup was accomplished using a mixed-mode solid-phase extraction. 9-Carboxy-ll-nor-A'-tetrahydroca
Simultaneous determination of Δ9-tetrahydrocannabinol, 11-hydroxy-Δ9-tetrahydrocannabinol and 11-nor-9-carboxy- Δ9-tetrahydrocannabinol in human plasma by high-performance liquid chromatography/tandem mass spectrometry
✍ Scribed by Barbora Maralikova; Wolfgang Weinmann
- Publisher
- John Wiley and Sons
- Year
- 2004
- Tongue
- English
- Weight
- 143 KB
- Volume
- 39
- Category
- Article
- ISSN
- 1076-5174
- DOI
- 10.1002/jms.616
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✦ Synopsis
Abstract
A rapid and sensitive method for the simultaneous confirmatory analysis of three forensic most relevant cannabinoids, Δ^9^‐tetrahydrocannabinol (THC), 11‐hydroxy‐Δ^9^‐tetrahydrocannabinol (11‐OH‐THC) and 11‐nor‐9‐carboxy‐Δ^9^‐tetrahydrocannabinol (THC‐COOH), by means of high‐performance liquid chromatography/tandem mass spectrometry (LC/MS/MS) in human plasma was developed and fully validated. Sample clean‐up was performed by automated silica‐based solid‐phase extraction and the separation was carried out using a PhenylHexyl column (50 × 2 mm i.d., 3 µm) and acetonitrile–5 mM ammonium acetate gradient elution. Data were acquired with an API 3000 LC/MS/MS system equipped with a turboionspray interface and triple quadrupole mass analyzer using positive electrospray ionization and multiple reaction monitoring. Two MS/MS transitions for each substance were monitored and deuterated analogues of analytes were used as internal standards for quantitation. The limit of quantitation was 0.8 ng ml^−1^ for THC, 0.8 ng ml^−1^ for 11‐OH‐THC and 4.3 ng ml^−1^ for THC‐COOH and linearity with a correlation coefficient r^2^ = 0.999 was achieved up to 100 ng ml^−1^ for THC and 11‐OH‐THC and 500 ng ml^−1^ for THC‐COOH. The limits of detection were 0.2 ng ml^−1^ for THC, 0.2 ng ml^−1^ for 11‐OH‐THC and 1.6 ng ml^−1^ for THC‐COOH. The developed LC/MS/MS method was also successfully used for the determination of THC‐COOH‐glucuronide, the phase II metabolite of THC‐COOH. Copyright © 2004 John Wiley & Sons, Ltd.
📜 SIMILAR VOLUMES
A gas chromatographic/mass spectrometric electron impact method is presented for the detection and quantification of 1 l-nor-9-carboxy-A9-tetrahydrocannabinol (THC-COOH) in urine, for use in the confirmation of presump tive results obtained by other techniques. Four extraction procedures, two solid-