Measurement Journal Issue 6

a positive test, a second aliquot of the A sample is taken and subjected to a more-detailed analysis. If this test is positive, the B sample is tested, but only after informing the athlete, who can be present and can also bring along their own expert observer. If the B sample generates a positive result, then the matter is referred to the anti-doping authority. No further action is taken if the B sample test is negative. Whatever the method, testing for sports doping places tremendous demands on analytical instruments. Above all, the equipment must be reliable because downtime is unacceptable, especially during a major event. The instrument must be able to process large numbers of samples in the lab with a rapid turnaround time: Those athletes being tested have a right to a prompt result. Day-to-day reproducibility is also crucial, particularly where conﬁrmatory analyses are concerned, to ensure conﬁdence in results that may be challenged. Applying appropriate tools and methods The optimal choice of analytical techniques and instruments varies depending on the target substance and the task (e.g., screening or conﬁrmation). As a general statement, GC is well suited to the separation of small, volatile compounds while LC is best for larger, non-volatile substances. In recent years, the utility of these separation techniques has been further expanded by the advent of robust tandem MS technologies such as LC or GC combined with a triple-quadrupole mass spectrometer (LC/QQQ and GC/QQQ). To be more speciﬁc, doping control labs typically use GC/NPD for screening of narcotics and some classes of stimulants, while GC/MS is used for broader screens including anabolic steroids, marijuana, marijuana metabolites, and opiates. Larger molecules, such as beta-blockers and glucocorticoids, are often screened for using tandem LC/MS. More recently, laboratories have been applying the rapid, full-scan capability of LC timeof-ﬂight (LC/TOF) and LC quadrupole time-of-ﬂight (LC/QTOF) to screen for presumptive positives. Because TOF instruments always operate in full-scan mode, which collects “all the data, all the time,” these technologies also provide laboratories with the ability to perform retrospective analysis. Immunoassays are used to screen for peptides and hormones such as human chorionic gonadotropin (hCG) and insulin. Isoelectric focusing (IEF) with chemiluminescence detection is used to screen for erythropoietin (EPO), which has become popular for boosting an athlete’s oxygen-carrying capacity. Conﬁrmation tests are often performed using GC/MS or some form of tandem LC/MS such as LC/QQQ. Recently, some have been using LC/MS ion-trap technology for target conﬁrmation due to its unique ability to generate multiple MS (MSn) spectra and provide a “spectral audit trail.” Similarly, some laboratories leverage the superb mass accuracy of LC/TOF or LC/QTOF to conﬁrm the presence of a target compound through empirical formula determination. Testing for steroids Steroids are the most commonly abused drugs because they increase muscle growth (mass) and decrease recovery time. More than 70 are on the banned list, the most common of which are stanozolol, testosterone, nandrolone, clenbuterol, and the new “designer steroid” tetrahydrogestrinone (THG) — but new ones are constantly emerging (Figure 2). H3C HO CH3 O Figure 2. Chemical structure of the designer steroid THG Honoring Excellence in Doping Control To underline its commitment to the ﬁeld, Agilent set up the Manfred Donike Award for scientiﬁc excellence in doping control in 1997. Professor Donike was a pioneer in doping tests, setting up one of the earliest dedicated labs in time for the Munich Games. The 2008 award went to Ulrich Flenker, a research scientist at the Institute of Biochemistry, German Sport University, Cologne, Germany. Flenker was honored for his continuous technical and scientiﬁc improvements in detecting doping with synthetic steroids by identifying the ratios of stable isotopes 13C to 12C in samples using gas chromatographycombustion-isotope ratio mass spectrometry (GC-C-IRMS). 13 Agilent Measurement Journal

Table of Contents Feed for the Digital Edition of Measurement Journal Issue 6

Measurement Journal Issue 6 Using a Few Words to Convey a Deeply-Held Spirit Charting a Unique Path to Technology Innovation Contents Announcing First Commercial GC/MS Metabolites Library Assessing Nonlinear Behavior Testing Combines Form and Function Testing Multiplay Networks Higher Sensitivity LC/MS Easing Military Radio Test Stepping Up Calibration Accuracy Increasing Spectrum Analyzer Bandwidth 3GPP Tool Supports TS 36 Standards The Olympic Story Spotlights Agilent's Continuing Contribution to Technology Innovation Ensuring a Level Playing Field in Competitive Sports GPS: Coming of Age Resolving Design Issues in HSPA Mobile Devices Achieving Accurate Results with Oscilloscope-Based Jitter-Analysis Software RF Handheld Testers Guarantee Traffic Stability Under Olympic-Sized Stress Conditions Utilizing LAN-Based Instrumentation to Measure Total Harmonic Distortion in Remote Facilities IMT-Advanced: 4G Wireless Takes Shape in an Olympic Year EPO Doping: A Speed Engine, Turbo-Charged by Chemistry

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