Ghent University Academic Bibliography

Advanced

Development and validation of an LC-MS/MS method for the quantification of ephedrines in urine

Koen Deventer UGent, Oscar Juan Pozo Mendoza UGent, Peter Van Eenoo UGent and Frans Delbeke UGent (2009) JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES. 877(4). p.369-374
abstract
The objective of this study was to develop a simple and robust LC-MS/MS method for the quantification of ephedrine type substances in urine. Sample preparation consisted of a 10-fold dilution step of the samples into the internal standard solution (ephedrine-d(3), 4 mu g/mL in water). Baseline separation of the diastereoisomers norpseudoephedrine-norephedrine and ephedrine-pseudoephedrine was performed On a C8-column using isocratic conditions followed by positive electrospray ionisation and tandem mass spectrometric detection. The mobile phase consisted of 98/2 (H2O/ACN) containing 0.1% HAc and 0.01% TFA. Calibration curves were constructed between 2.5 and 10 mu g/mL for norephedrine and norpseudoephedrine and 5 and 20 mu g/mL for ephedrine, pseudoephedrine and methylephedrine. The bias ranged from -5.5 to 12% for norephedrine, -4.1 to 8.0% for norpseudoephedrine, 0.3 to 2.1% for ephedrine,1.6 to 2.6% for pseudoephedrine and 2.9 to 5.0% for methylephedrine. Precision of the method varied between 2.8 and 10.4% for all compounds and the matrix effect was less than 15%. The applicability of the method has been checked by the analysis of 40 urine samples. The results were compared with those obtained with the common GC-NPD method. Results show a good correlation between both methods with correlation coefficients higher than 0.95 for all analytes. (C) 2009 Elsevier B.V. All rights reserved.
Please use this url to cite or link to this publication:
author
organization
year
type
journalArticle (original)
publication status
published
subject
keyword
Doping, DRUGS, TRAP MASS-SPECTROMETRY, ELECTROSPRAY-IONIZATION, Urine, Ephedrine, Amphetamine, AGENTS, Mass spectrometry, PERFORMANCE LIQUID-CHROMATOGRAPHY, DOPING CONTROL ANALYSIS, Sport
journal title
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
J. Chromatogr. B
volume
877
issue
4
pages
369 - 374
publisher
Elsevier Science
place of publication
PO BOX 211, 1000 AE AMSTERDAM, NETHERLANDS
Web of Science type
Article
Web of Science id
000263190900002
JCR category
CHEMISTRY, ANALYTICAL
JCR impact factor
2.777 (2009)
JCR rank
14/70 (2009)
JCR quartile
1 (2009)
ISSN
1570-0232
DOI
10.1016/j.jchromb.2008.12.032
language
English
UGent publication?
yes
classification
A1
id
714136
handle
http://hdl.handle.net/1854/LU-714136
date created
2009-07-06 10:48:29
date last changed
2009-07-28 15:22:48
@article{714136,
  abstract     = {The objective of this study was to develop a simple and robust LC-MS/MS method for the quantification of ephedrine type substances in urine. Sample preparation consisted of a 10-fold dilution step of the samples into the internal standard solution (ephedrine-d(3), 4 mu g/mL in water). Baseline separation of the diastereoisomers norpseudoephedrine-norephedrine and ephedrine-pseudoephedrine was performed On a C8-column using isocratic conditions followed by positive electrospray ionisation and tandem mass spectrometric detection. The mobile phase consisted of 98/2 (H2O/ACN) containing 0.1\% HAc and 0.01\% TFA. Calibration curves were constructed between 2.5 and 10 mu g/mL for norephedrine and norpseudoephedrine and 5 and 20 mu g/mL for ephedrine, pseudoephedrine and methylephedrine. The bias ranged from -5.5 to 12\% for norephedrine, -4.1 to 8.0\% for norpseudoephedrine, 0.3 to 2.1\% for ephedrine,1.6 to 2.6\% for pseudoephedrine and 2.9 to 5.0\% for methylephedrine. Precision of the method varied between 2.8 and 10.4\% for all compounds and the matrix effect was less than 15\%. The applicability of the method has been checked by the analysis of 40 urine samples. The results were compared with those obtained with the common GC-NPD method. Results show a good correlation between both methods with correlation coefficients higher than 0.95 for all analytes. (C) 2009 Elsevier B.V. All rights reserved.},
  author       = {Deventer, Koen and Pozo Mendoza, Oscar Juan and Van Eenoo, Peter and Delbeke, Frans},
  issn         = {1570-0232},
  journal      = {JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES},
  keyword      = {Doping,DRUGS,TRAP MASS-SPECTROMETRY,ELECTROSPRAY-IONIZATION,Urine,Ephedrine,Amphetamine,AGENTS,Mass spectrometry,PERFORMANCE LIQUID-CHROMATOGRAPHY,DOPING CONTROL ANALYSIS,Sport},
  language     = {eng},
  number       = {4},
  pages        = {369--374},
  publisher    = {Elsevier Science},
  title        = {Development and validation of an LC-MS/MS method for the quantification of ephedrines in urine},
  url          = {http://dx.doi.org/10.1016/j.jchromb.2008.12.032},
  volume       = {877},
  year         = {2009},
}

Chicago
Deventer, Koen, Oscar Juan Pozo Mendoza, Peter Van Eenoo, and Frans Delbeke. 2009. “Development and Validation of an LC-MS/MS Method for the Quantification of Ephedrines in Urine.” Journal of Chromatography B-analytical Technologies in the Biomedical and Life Sciences 877 (4): 369–374.
APA
Deventer, K., Pozo Mendoza, O. J., Van Eenoo, P., & Delbeke, F. (2009). Development and validation of an LC-MS/MS method for the quantification of ephedrines in urine. JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES, 877(4), 369–374.
Vancouver
1.
Deventer K, Pozo Mendoza OJ, Van Eenoo P, Delbeke F. Development and validation of an LC-MS/MS method for the quantification of ephedrines in urine. JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES. PO BOX 211, 1000 AE AMSTERDAM, NETHERLANDS: Elsevier Science; 2009;877(4):369–74.
MLA
Deventer, Koen, Oscar Juan Pozo Mendoza, Peter Van Eenoo, et al. “Development and Validation of an LC-MS/MS Method for the Quantification of Ephedrines in Urine.” JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES 877.4 (2009): 369–374. Print.