Screening and confirmation capabilities of liquid chromatography-time-of-flight mass spectrometry for the determination of 200 multiclass sport drugs in urine

Development of a multi‐functional concurrent assay using weak cation‐exchange solid‐phase extraction (WCX‐SPE) and reconstitution with a diluted sample aliquot for anti‐doping analysis

“…Liquid chromatography/tandem mass spectrometry (LC/MS/MS) is now extensively utilized due to its high selectivity and sensitivity. In addition, many doping analyses are conducted using various extraction methodologies, such as liquid–liquid extraction (LLE), protein precipitation (PP), or solid‐phase extraction (SPE) . SPE presents several advantages over LLE or PP because it includes a relatively simple pre‐treatment procedure and is less dependent on the proficiency of the researcher.…”

“…In addition, many doping analyses are conducted using various extraction methodologies, such as liquidliquid extraction (LLE), protein precipitation (PP), or solid-phase extraction (SPE). [3][4][5][6][7][8][9][10][11] SPE presents several advantages over LLE or PP because it includes a relatively simple pre-treatment procedure and is less dependent on the proficiency of the researcher. Moreover, it involves less sample manipulation, which should provide good reproducibility and thus higher sensitivity and selectivity.…”

Annual banned‐substance review: analytical approaches in human sports drug testing

“…Using SPE of urine followed by reversed-phase LC-time-of-flight (TOF) MS, a subset of 32 AAS-related analytes was determined from human urine as part of an extensive initial testing method covering a total 200 drug analytes published by Dominguez-Romero et al [62] While the accomplished LODs were adequate, it remained unclear how the commonly glucuronic acid-or sulfate-conjugated steroid metabolites are detected in authentic scenarios in the absence of a sample preparation step enabling the hydrolysis of commonly excreted phase II metabolites. Moreover, the lack of internal standards appeared inappropriate for human sports drug testing, raising substantial concerns about the fitness-for-purpose of this approach.…”

Methods for Doping Detection

“…m/z 95-1,000) with a broad dynamic range, highly accurate measurement of mass, and high sensitivity. Modern TOF/MS and tandem QTOF/MS instruments have performances comparable to that of the Orbitrap, but faster acquisition speeds (up to 100 Hz) [16] . However, in contrast to Orbitrap technology, working at very high resolution (up to 80,000 full width at half maximum) impacts detection sensitivity.…”