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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)
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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.
Keywords
Doping, DRUGS, TRAP MASS-SPECTROMETRY, ELECTROSPRAY-IONIZATION, Urine, Ephedrine, Amphetamine, AGENTS, Mass spectrometry, PERFORMANCE LIQUID-CHROMATOGRAPHY, DOPING CONTROL ANALYSIS, Sport

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MLA
Deventer, Koen 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.
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.
Chicago author-date
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.
Chicago author-date (all authors)
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.
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.
IEEE
[1]
K. Deventer, O. J. Pozo Mendoza, P. Van Eenoo, and F. Delbeke, “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, vol. 877, no. 4, pp. 369–374, 2009.
@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},
  keywords     = {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},
}

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