The Determination of Cocaine, Benzoylecgonine, and Cocaethylene in Small-Volume Oral Fluid Samples by Liquid Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry

A quantitative analysis was developed for the determination of cocaine, benzoylecgonine, and cocaethylene in oral fluid using liquid chromatography-tandem mass spectrometry. After internal standardization and solid-phase extraction, chromatographic separation was achieved on a reversed-phase column...

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Bibliographic Details
Published in:Journal of analytical toxicology 2004-11, Vol.28 (8), p.655-659
Main Authors: Clauwaert, K., Decaestecker, T., Mortier, K., Lambert, W., Deforce, D., Van Peteghem, C., Van Bocxlaer, J.
Format: Article
Language:English
Subjects:
Analysis
Biological and medical sciences
Chromatography, Liquid - methods
Cocaine - analogs & derivatives
Cocaine - analysis
Cocaine-Related Disorders - diagnosis
Cocaine-Related Disorders - metabolism
Drug addictions
General pharmacology
Humans
Medical sciences
Pharmacology. Drug treatments
Reproducibility of Results
Saliva - chemistry
Spectrometry, Mass, Electrospray Ionization - methods
Substance Abuse Detection - methods
Toxicology
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Summary:A quantitative analysis was developed for the determination of cocaine, benzoylecgonine, and cocaethylene in oral fluid using liquid chromatography-tandem mass spectrometry. After internal standardization and solid-phase extraction, chromatographic separation was achieved on a reversed-phase column by gradient elution. The reconstructed mass chromatograms of the collision-induced dissociation transitions of m/z 290 → m/z 168 (benzoylecgonine), m/z 304 → m/z 168+119 (2′-methylbenzoylecgonine), m/z 304 → m/z 182 (cocaine), m/z 318 → m/z 196 (cocaethylene), and m/z 318 → m/z 182+119 (2′-methylcocaine) were used for quantitation. The developed method was adequately validated. Good linearity was obtained from 10 to 1000 µg/L. Extraction recoveries exceeded 85 % for all compounds. Excellent total and within-run reproducibilities (CV% < 20%) and accuracy figures were obtained. The limit of detection (signal-to-noise ratio ≥ 3) was 1 µg/L for all three compounds. As such, a method for drug abuse confirmation analysis in oral fluid, compatible with the present day saliva collecting devices, is obtained. The method was applied to real samples (n = 15) obtained from suspected drug users, of which seven proved positive. The concentrations found in the positive samples were between 10.2 and 200.6 µg/L for cocaine, < limit of quantification (LOQ) and 10.5 µg/L for cocaethylene, and < LOQ and 59.2 µg/L for benzoylecgonine.
ISSN:0146-4760
1945-2403
DOI:10.1093/jat/28.8.655