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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.
J Chromatogr A. 2009 Jul 31; 1216(31):5819-27.JC

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.

Authors+Show Affiliations

Doping control laboratory (DoCoLab), Ghent University (UGent), Department of Clinical Chemistry, Microbiology and Immunology, Technologiepark 30, B-9052 Zwijnaarde, Belgium. Koen.Deventer@UGent.beNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

19560151

Citation

Deventer, K, 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, vol. 1216, no. 31, 2009, pp. 5819-27.
Deventer K, Pozo OJ, Van Eenoo P, 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. J Chromatogr A. 2009;1216(31):5819-27.
Deventer, K., Pozo, O. J., Van Eenoo, P., & Delbeke, F. T. (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), 5819-27. https://doi.org/10.1016/j.chroma.2009.06.003
Deventer K, 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. J Chromatogr A. 2009 Jul 31;1216(31):5819-27. PubMed PMID: 19560151.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - 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. AU - Deventer,K, AU - Pozo,O J, AU - Van Eenoo,P, AU - Delbeke,F T, Y1 - 2009/06/07/ PY - 2009/02/02/received PY - 2009/05/29/revised PY - 2009/06/02/accepted PY - 2009/6/30/entrez PY - 2009/6/30/pubmed PY - 2009/9/25/medline SP - 5819 EP - 27 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1216 IS - 31 N2 - 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. SN - 1873-3778 UR - https://www.unboundmedicine.com/medline/citation/19560151/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_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(09)00866-8 DB - PRIME DP - Unbound Medicine ER -