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Qualitative detection of diuretics and acidic metabolites of other doping agents in human urine by high-performance liquid chromatography-tandem mass spectrometry Comparison between liquid-liquid extraction and direct injection

Koen Deventer UGent, Oscar Juan Pozo Mendoza UGent, Peter Van Eenoo UGent and Frans Delbeke UGent (2009) JOURNAL OF CHROMATOGRAPHY A. 1216(31). p.5819-5827
abstract
Direct injection of urine has gained interest in the field of analytical toxicology, including doping control analysis. However, implementation of a direct urinalysis method for the LC-MS/MS detection of 34 diuretics and 9 other doping agents yielded several analytical problems, which were not observed using a traditional liquid-liquid extraction. Therefore a comparative study was made between liquid-liquid extraction and direct injection. Comparison of validation results showed that the liquid-liquid extraction at pH 7 allows to analyze samples without major drawbacks regarding matrix effects. Hence, good sensitivity was observed and detection limits ranged between 1 and 250 ng/mL for all compounds. In the direct injection approach shifted retention times were observed for several acidic and basic compounds due to unwanted matrix effects. This shift was reduced by a 25-fold dilution of the urine samples. Besides the improved retention time stability the diluted samples also exhibited lower ion suppression than the undiluted ones. After 25-fold dilution, detection limits ranged between 10 and 250 ng/mL for all compounds. Since these detection limits are at or below the minimum required performance level, imposed by the World Anti-Doping Agency, the method could be applied to routine anti-doping analysis. Samples, previously declared positive, were reanalysed using both the liquid-liquid extraction and direct injection. With both techniques all 26 samples were found to be positive, showing the applicability of direct injection for the analysis of diuretics. (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
MS/MS, IONIZATION, STIMULANTS, EPHEDRINES, QUANTIFICATION, HIGH-THROUGHPUT, ANABOLIC-STEROIDS, SCREENING METHOD, Urine, SOLID-PHASE EXTRACTION, Ion suppression, Sports, Diuretics, Direct injection, Mass spectrometry, Doping, Liquid-chromatography
journal title
JOURNAL OF CHROMATOGRAPHY A
J. Chromatogr. A
volume
1216
issue
31
pages
5819 - 5827
publisher
Elsevier Science
place of publication
PO BOX 211, 1000 AE AMSTERDAM, NETHERLANDS
Web of Science id
000268353200005
JCR category
CHEMISTRY, ANALYTICAL
JCR impact factor
4.101 (2009)
JCR rank
4/70 (2009)
JCR quartile
1 (2009)
ISSN
0021-9673
DOI
10.1016/j.chroma.2009.06.003
isi:typeArticle
language
English
UGent publication?
yes
classification
A1
id
737641
handle
http://hdl.handle.net/1854/LU-737641
date created
2009-09-01 10:34:16
date last changed
2009-09-07 11:54:11
@article{737641,
  abstract     = {Direct injection of urine has gained interest in the field of analytical toxicology, including doping control analysis. However, implementation of a direct urinalysis method for the LC-MS/MS detection of 34 diuretics and 9 other doping agents yielded several analytical problems, which were not observed using a traditional liquid-liquid extraction. Therefore a comparative study was made between liquid-liquid extraction and direct injection. Comparison of validation results showed that the liquid-liquid extraction at pH 7 allows to analyze samples without major drawbacks regarding matrix effects. Hence, good sensitivity was observed and detection limits ranged between 1 and 250 ng/mL for all compounds. In the direct injection approach shifted retention times were observed for several acidic and basic compounds due to unwanted matrix effects. This shift was reduced by a 25-fold dilution of the urine samples. Besides the improved retention time stability the diluted samples also exhibited lower ion suppression than the undiluted ones. After 25-fold dilution, detection limits ranged between 10 and 250 ng/mL for all compounds. Since these detection limits are at or below the minimum required performance level, imposed by the World Anti-Doping Agency, the method could be applied to routine anti-doping analysis. Samples, previously declared positive, were reanalysed using both the liquid-liquid extraction and direct injection. With both techniques all 26 samples were found to be positive, showing the applicability of direct injection for the analysis of diuretics. (C) 2009 Elsevier B.V. All rights reserved.},
  author       = {Deventer, Koen and Pozo Mendoza, Oscar Juan and Van Eenoo, Peter and Delbeke, Frans},
  issn         = {0021-9673},
  journal      = {JOURNAL OF CHROMATOGRAPHY A},
  keyword      = {MS/MS,IONIZATION,STIMULANTS,EPHEDRINES,QUANTIFICATION,HIGH-THROUGHPUT,ANABOLIC-STEROIDS,SCREENING METHOD,Urine,SOLID-PHASE EXTRACTION,Ion suppression,Sports,Diuretics,Direct injection,Mass spectrometry,Doping,Liquid-chromatography},
  language     = {eng},
  number       = {31},
  pages        = {5819--5827},
  publisher    = {Elsevier Science},
  title        = {Qualitative detection of diuretics and acidic metabolites of other doping agents in human urine by high-performance liquid chromatography-tandem mass spectrometry Comparison between liquid-liquid extraction and direct injection},
  url          = {http://dx.doi.org/10.1016/j.chroma.2009.06.003},
  volume       = {1216},
  year         = {2009},
}

Chicago
Deventer, Koen, Oscar Juan Pozo Mendoza, Peter Van Eenoo, and Frans Delbeke. 2009. “Qualitative Detection of Diuretics and Acidic Metabolites of Other Doping Agents in Human Urine by High-performance Liquid Chromatography-tandem Mass Spectrometry Comparison Between Liquid-liquid Extraction and Direct Injection.” Journal of Chromatography A 1216 (31): 5819–5827.
APA
Deventer, K., Pozo Mendoza, O. J., Van Eenoo, P., & Delbeke, F. (2009). Qualitative detection of diuretics and acidic metabolites of other doping agents in human urine by high-performance liquid chromatography-tandem mass spectrometry Comparison between liquid-liquid extraction and direct injection. JOURNAL OF CHROMATOGRAPHY A, 1216(31), 5819–5827.
Vancouver
1.
Deventer K, Pozo Mendoza OJ, Van Eenoo P, Delbeke F. Qualitative detection of diuretics and acidic metabolites of other doping agents in human urine by high-performance liquid chromatography-tandem mass spectrometry Comparison between liquid-liquid extraction and direct injection. JOURNAL OF CHROMATOGRAPHY A. PO BOX 211, 1000 AE AMSTERDAM, NETHERLANDS: Elsevier Science; 2009;1216(31):5819–27.
MLA
Deventer, Koen, Oscar Juan Pozo Mendoza, Peter Van Eenoo, et al. “Qualitative Detection of Diuretics and Acidic Metabolites of Other Doping Agents in Human Urine by High-performance Liquid Chromatography-tandem Mass Spectrometry Comparison Between Liquid-liquid Extraction and Direct Injection.” JOURNAL OF CHROMATOGRAPHY A 1216.31 (2009): 5819–5827. Print.