title: Use of ultra-high pressure liquid chromatography coupled to high resolution mass spectrometry for fast screening in high throughput doping control.
abstract: We describe a sensitive, comprehensive and fast screening method based on liquid chromatography-high resolution mass spectrometry for the detection of a large number of analytes in sports samples. UHPLC coupled to high resolution mass spectrometry with polarity switching capability is applied for the rapid screening of a large number of analytes in human urine samples. Full scan data are acquired alternating both positive and negative ionisation. Collision-induced dissociation with positive ionisation is also performed to produce fragment ions to improve selectivity for some analytes. Data are reviewed as extracted ion chromatograms based on narrow mass/charge windows (±5ppm). A simple sample preparation method was developed, using direct enzymatic hydrolysis of glucuronide conjugates, followed by solid phase extraction with mixed mode ion-exchange cartridges. Within a 10min run time (including re-equilibration) the method presented allows for the analysis of a large number of analytes from most of the classes in the World Anti-Doping Agency (WADA) Prohibited List, including anabolic agents, β2-agonists, hormone antagonists and modulators, diuretics, stimulants, narcotics, glucocorticoids and β-blockers, and does so while meeting the WADA sensitivity requirements. The high throughput of the method and the fast sample pre-treatment reduces analysis cost and increases productivity. The method presented has been used for the analysis of over 5000 samples in about one month and proved to be reliable.
authors.affiliation: Drug Control Centre, King's College London, London SE1 9NH, UK.
authors.forename: Alessandro
authors.initials: A
authors.lastname: Musenga
authors.forename: David A
authors.initials: DA
authors.lastname: Cowan
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004300:Doping in Sports; D057166:High-Throughput Screening Assays / Q000379:methods*; D006801:Humans; D057230:Limit of Detection; D013058:Mass Spectrometry / Q000379:methods*; D004364:Pharmaceutical Preparations / Q000737:chemistry / Q000652:urine*; D015203:Reproducibility of Results
chemical_list: D004364:Pharmaceutical Preparations