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High-throughput and sensitive screening by ultra-performance liquid chromatography tandem mass spectrometry of diuretics and other doping agents.
Eur J Mass Spectrom (Chichester). 2008; 14(3):191-200.EJ

Abstract

The reliability of ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC- MS/MS) for high throughput screening in anti-doping control has been tested. A method to screen for the presence of diuretics and other doping agents in urine has been optimised and validated. The extraction procedure consisted of an alkaline extraction (pH 9.5) with ethyl acetate and salting-out effect (sodium chloride). The extracts were analysed by UPLC-MS/MS. Analysis of 34 forbidden drugs and metabolites was achieved in a total run time of 5 min, using a C18 column (100 mm x 2.1 mm i.d., 1.7 microm particle size) and a mobile phase containing deionised water and acetonitrile with formic acid, with gradient elution at a flow-rate of 0.6 mL min(-1). Identification of the compounds was performed by multiple reaction monitoring, using electrospray ionisation in positive- or negative-ion mode. Precursor and product ions were studied for each compound and cone voltage and collision energy were optimised. Due to the different chemical structure of the compounds under study, extraction recoveries varied from less than 10% to 100% depending on the analyte. The limits of detection ranged from 50 ng mL(-1) to 200 ng mL(-1), and all the compounds comply with the requirements of quality established by the World Anti-doping Agency. Intra-assay precision was evaluated at two concentrations for each compound and, in most cases, a relative standard deviation of the signal ratio lower than 20% was obtained. The method has demonstrated to be reliable when analysing routine samples and the short analysis time resulting from a simple sample preparation and a rapid instrumental analysis allow a fast turn-around time and makes it of great interest for routine anti-doping control purposes.

Authors+Show Affiliations

Grup de Recerca en Bioanàlisis, IMIM-Hospital del Mar, Barcelona, Spain. rventura@imim.esNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

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

Language

eng

PubMed ID

18708699

Citation

Ventura, Rosa, et al. "High-throughput and Sensitive Screening By Ultra-performance Liquid Chromatography Tandem Mass Spectrometry of Diuretics and Other Doping Agents." European Journal of Mass Spectrometry (Chichester, England), vol. 14, no. 3, 2008, pp. 191-200.
Ventura R, Roig M, Montfort N, et al. High-throughput and sensitive screening by ultra-performance liquid chromatography tandem mass spectrometry of diuretics and other doping agents. Eur J Mass Spectrom (Chichester). 2008;14(3):191-200.
Ventura, R., Roig, M., Montfort, N., Sáez, P., Bergés, R., & Segura, J. (2008). High-throughput and sensitive screening by ultra-performance liquid chromatography tandem mass spectrometry of diuretics and other doping agents. European Journal of Mass Spectrometry (Chichester, England), 14(3), 191-200. https://doi.org/10.1255/ejms.920
Ventura R, et al. High-throughput and Sensitive Screening By Ultra-performance Liquid Chromatography Tandem Mass Spectrometry of Diuretics and Other Doping Agents. Eur J Mass Spectrom (Chichester). 2008;14(3):191-200. PubMed PMID: 18708699.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - High-throughput and sensitive screening by ultra-performance liquid chromatography tandem mass spectrometry of diuretics and other doping agents. AU - Ventura,Rosa, AU - Roig,M, AU - Montfort,N, AU - Sáez,P, AU - Bergés,Rosa, AU - Segura,Jordi, PY - 2008/8/19/pubmed PY - 2008/9/24/medline PY - 2008/8/19/entrez SP - 191 EP - 200 JF - European journal of mass spectrometry (Chichester, England) JO - Eur J Mass Spectrom (Chichester) VL - 14 IS - 3 N2 - The reliability of ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC- MS/MS) for high throughput screening in anti-doping control has been tested. A method to screen for the presence of diuretics and other doping agents in urine has been optimised and validated. The extraction procedure consisted of an alkaline extraction (pH 9.5) with ethyl acetate and salting-out effect (sodium chloride). The extracts were analysed by UPLC-MS/MS. Analysis of 34 forbidden drugs and metabolites was achieved in a total run time of 5 min, using a C18 column (100 mm x 2.1 mm i.d., 1.7 microm particle size) and a mobile phase containing deionised water and acetonitrile with formic acid, with gradient elution at a flow-rate of 0.6 mL min(-1). Identification of the compounds was performed by multiple reaction monitoring, using electrospray ionisation in positive- or negative-ion mode. Precursor and product ions were studied for each compound and cone voltage and collision energy were optimised. Due to the different chemical structure of the compounds under study, extraction recoveries varied from less than 10% to 100% depending on the analyte. The limits of detection ranged from 50 ng mL(-1) to 200 ng mL(-1), and all the compounds comply with the requirements of quality established by the World Anti-doping Agency. Intra-assay precision was evaluated at two concentrations for each compound and, in most cases, a relative standard deviation of the signal ratio lower than 20% was obtained. The method has demonstrated to be reliable when analysing routine samples and the short analysis time resulting from a simple sample preparation and a rapid instrumental analysis allow a fast turn-around time and makes it of great interest for routine anti-doping control purposes. SN - 1469-0667 UR - https://www.unboundmedicine.com/medline/citation/18708699/High_throughput_and_sensitive_screening_by_ultra_performance_liquid_chromatography_tandem_mass_spectrometry_of_diuretics_and_other_doping_agents_ DB - PRIME DP - Unbound Medicine ER -