Simultaneous analysis of 210 prohibited substances in human urine by ultrafast liquid chromatography/tandem mass spectrometry in doping control

Abstract

A multiresidue analytical method was developed and validated for screening and confirming the presence of performance-enhancing drugs. A total of 210 substances from diverse classes of prohibited substances were successfully identified with an analytical run time of 10 min.

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

“…To evaluate the sensitivity of the developed method, we compared it with the previous in‐house methodologies . Even if the assays were performed under different chromatographic and mass spectrometric conditions, we were still able to appraise the sensitivity of our novel method with some degree of certainty.…”

“…The potassium carbonate solution was produced by dissolving 50 g of potassium carbonate in 1000 mL of water. 95 mL of 0.1 M citric acid and 415 mL of 0.1 M sodium citrate were diluted with water to obtain a final volume of 1000 mL, and 2 mL of 5 N potassium hydroxide was added to adjust the pH to 6.0 …”

“…An internal standard mixture (10 μL, ISTD), 700 μL of 0.1 M citrate buffer, and 50 μL of β‐glucuronidase/arylsulfatase were added to the remaining sample volume of 1960 μL. Hydrolysis was performed according to the previously established in‐house methodologies . The SPE cartridge was washed using 2 mL of methanol and was conditioned with 2 mL of water.…”

“…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.…”