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Fast analysis of doping agents in urine by ultra-high-pressure liquid chromatography-quadrupole time-of-flight mass spectrometry I. Screening analysis.
J Chromatogr A. 2009 May 15; 1216(20):4423-33.JC

Abstract

The general strategy to perform anti-doping analyses of urine samples starts with the screening for a wide range of compounds. This step should be fast, generic and able to detect any sample that may contain a prohibited substance while avoiding false negatives and reducing false positive results. The experiments presented in this work were based on ultra-high-pressure liquid chromatography coupled to hybrid quadrupole time-of-flight mass spectrometry. Thanks to the high sensitivity of the method, urine samples could be diluted 2-fold prior to injection. One hundred and three forbidden substances from various classes (such as stimulants, diuretics, narcotics, anti-estrogens) were analysed on a C(18) reversed-phase column in two gradients of 9min (including two 3min equilibration periods) for positive and negative electrospray ionisation and detected in the MS full scan mode. The automatic identification of analytes was based on retention time and mass accuracy, with an automated tool for peak picking. The method was validated according to the International Standard for Laboratories described in the World Anti-Doping Code and was selective enough to comply with the World Anti-Doping Agency recommendations. In addition, the matrix effect on MS response was measured on all investigated analytes spiked in urine samples. The limits of detection ranged from 1 to 500ng/mL, allowing the identification of all tested compounds in urine. When a sample was reported positive during the screening, a fast additional pre-confirmatory step was performed to reduce the number of confirmatory analyses.

Authors+Show Affiliations

Swiss Anti Doping Laboratory, University Center of Legal Medicine, Geneva and Lausanne, Chemin des Croisettes 22, 1066 Epalinges, Switzerland.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Evaluation Study
Journal Article

Language

eng

PubMed ID

19342059

Citation

Badoud, F, et al. "Fast Analysis of Doping Agents in Urine By Ultra-high-pressure Liquid Chromatography-quadrupole Time-of-flight Mass Spectrometry I. Screening Analysis." Journal of Chromatography. A, vol. 1216, no. 20, 2009, pp. 4423-33.
Badoud F, Grata E, Perrenoud L, et al. Fast analysis of doping agents in urine by ultra-high-pressure liquid chromatography-quadrupole time-of-flight mass spectrometry I. Screening analysis. J Chromatogr A. 2009;1216(20):4423-33.
Badoud, F., Grata, E., Perrenoud, L., Avois, L., Saugy, M., Rudaz, S., & Veuthey, J. L. (2009). Fast analysis of doping agents in urine by ultra-high-pressure liquid chromatography-quadrupole time-of-flight mass spectrometry I. Screening analysis. Journal of Chromatography. A, 1216(20), 4423-33. https://doi.org/10.1016/j.chroma.2009.03.033
Badoud F, et al. Fast Analysis of Doping Agents in Urine By Ultra-high-pressure Liquid Chromatography-quadrupole Time-of-flight Mass Spectrometry I. Screening Analysis. J Chromatogr A. 2009 May 15;1216(20):4423-33. PubMed PMID: 19342059.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Fast analysis of doping agents in urine by ultra-high-pressure liquid chromatography-quadrupole time-of-flight mass spectrometry I. Screening analysis. AU - Badoud,F, AU - Grata,E, AU - Perrenoud,L, AU - Avois,L, AU - Saugy,M, AU - Rudaz,S, AU - Veuthey,J-L, Y1 - 2009/03/18/ PY - 2009/01/13/received PY - 2009/03/03/revised PY - 2009/03/13/accepted PY - 2009/4/4/entrez PY - 2009/4/4/pubmed PY - 2009/7/3/medline SP - 4423 EP - 33 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1216 IS - 20 N2 - The general strategy to perform anti-doping analyses of urine samples starts with the screening for a wide range of compounds. This step should be fast, generic and able to detect any sample that may contain a prohibited substance while avoiding false negatives and reducing false positive results. The experiments presented in this work were based on ultra-high-pressure liquid chromatography coupled to hybrid quadrupole time-of-flight mass spectrometry. Thanks to the high sensitivity of the method, urine samples could be diluted 2-fold prior to injection. One hundred and three forbidden substances from various classes (such as stimulants, diuretics, narcotics, anti-estrogens) were analysed on a C(18) reversed-phase column in two gradients of 9min (including two 3min equilibration periods) for positive and negative electrospray ionisation and detected in the MS full scan mode. The automatic identification of analytes was based on retention time and mass accuracy, with an automated tool for peak picking. The method was validated according to the International Standard for Laboratories described in the World Anti-Doping Code and was selective enough to comply with the World Anti-Doping Agency recommendations. In addition, the matrix effect on MS response was measured on all investigated analytes spiked in urine samples. The limits of detection ranged from 1 to 500ng/mL, allowing the identification of all tested compounds in urine. When a sample was reported positive during the screening, a fast additional pre-confirmatory step was performed to reduce the number of confirmatory analyses. SN - 1873-3778 UR - https://www.unboundmedicine.com/medline/citation/19342059/Fast_analysis_of_doping_agents_in_urine_by_ultra_high_pressure_liquid_chromatography_quadrupole_time_of_flight_mass_spectrometry_I__Screening_analysis_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(09)00431-2 DB - PRIME DP - Unbound Medicine ER -