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Published on: April 23, 2019
Introduction of HPLC/orbitrap mass spectrometry as screening method for doping control
E D Virus1, T G Sobolevsky, G M Rodchenkov
1Moscow Antidoping Center, Elizavetynsky10, 105005, Moscow, Russia. virus@dopingcontrol.ru
Journal of Mass Spectrometry : JMS
|June 20, 2008
Summary
A new HPLC/orbitrap method enhances doping control by detecting 29 agents in urine. This sensitive screening tool offers high accuracy and low detection limits for antiestrogenic agents, anabolic steroids, and more.
Area of Science:
- Analytical Chemistry
- Forensic Science
- Biochemistry
Background:
- Doping control relies on sensitive and accurate analytical methods for detecting prohibited substances in athletes' biological samples.
- Existing methods may face limitations in sensitivity, specificity, or the range of detectable compounds.
- Advancements in mass spectrometry offer potential for improved doping analysis.
Purpose of the Study:
- To develop and validate a novel high-performance liquid chromatography/orbitrap mass spectrometry (HPLC/Orbitrap) method for doping control.
- To enable the simultaneous detection of a wide array of doping agents in human urine samples.
- To establish the method's performance characteristics, including accuracy, sensitivity, and precision.
Main Methods:
- Utilized HPLC coupled with Orbitrap mass spectrometry, employing in-source collision-induced dissociation (ISCID) and atmospheric pressure chemical ionization (APCI).
- Screened for 29 doping compounds, encompassing antiestrogenic agents, beta(2) agonists, and exogenous anabolic steroids.
- Validated analytical performance metrics such as mass accuracy, limit of detection (LOD), analyte recovery, repeatability, and precision.
Main Results:
- Achieved excellent mass accuracy (<2 ppm) with an external reference standard.
- Demonstrated a sensitive detection limit below 100 pg/ml for all tested compounds.
- Reported high analyte recoveries (>70%) and robust precision, with median repeatability values of 21% at 1 ng/ml and 17% at 10 ng/ml.
- Intraday precision ranged from 16-22% RSD, and interday precision ranged from 17-26% RSD.
Conclusions:
- The developed HPLC/Orbitrap method is a powerful tool for doping control, offering sensitive and accurate detection of diverse prohibited substances.
- The method's performance characteristics meet the stringent requirements for anti-doping laboratories.
- This advancement contributes to more effective WADA (World Anti-Doping Agency) compliance and athlete integrity in sports.
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