Document Detail

Rapid and robust confirmation and quantification of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid (THC-COOH) in urine by column switching LC-MS-MS analysis.
MedLine Citation:
PMID:  22282098     Owner:  NLM     Status:  In-Data-Review    
A method for the rapid and robust confirmation of 11-nor-∆9-tetrahydrocannabinol-9-carboxylic acid (THCA) in urine involving basic hydrolysis with NaOH and direct injection of the hydrolysate in a column-switching LC-MS-MS system was developed and validated. THCA-d3 was used as internal standard. Detection was performed in negative-ion mode by monitoring the transitions from the [M-CO(2) ]- ion m/z 299.2→245.2 and and m/z 299.2→191.1 that were found to provide a better signal-to-noise ratio than the transition from the pseudomolecular ion at m/z 343. The high sensitivity of detection enabled the injection of a small volume (10 µl) of the NaOH hydrolysate which, together with the applied column switching system, proved to confer ruggedness to the method and to avoid the deterioration of the instrumental apparatus despite the large amount of inorganic ions in the hydrolysate. The LLOQ was established at 5 ng/ml, and the LLOD was calculated as 0.2 ng/ml (S/N =3). The method was submitted to thorough validation including evaluation of the calibration range (5-500 ng/ml), accuracy and precision, matrix effects, overall process efficiency, autosampler stability, carryover and cross-talk, and 10-times reduction of sample volume (0.1 ml). Proof of applicability was obtained by direct comparison with the reference GC-MS method in use in the lab (the R(2) between the two methods was 0.9951). Copyright © 2012 John Wiley & Sons, Ltd.
Gabriele Zanchetti; Ivan Floris; Alberto Piccinotti; Silvia Tameni; Aldo Polettini
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Publication Detail:
Type:  Journal Article    
Journal Detail:
Title:  Journal of mass spectrometry : JMS     Volume:  47     ISSN:  1096-9888     ISO Abbreviation:  J Mass Spectrom     Publication Date:  2012 Jan 
Date Detail:
Created Date:  2012-01-27     Completed Date:  -     Revised Date:  -    
Medline Journal Info:
Nlm Unique ID:  9504818     Medline TA:  J Mass Spectrom     Country:  England    
Other Details:
Languages:  eng     Pagination:  124-30     Citation Subset:  IM    
Copyright Information:
Copyright © 2012 John Wiley & Sons, Ltd.
Synlab Italia Srl, Brescia, Italy.
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