Developing a reference measurement procedure for free glycerol in human serum by two-step gas chromatography–isotope dilution mass spectrometry

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

“…[33] Its metabolism was studied by Cox et al, who incubated the analyte in human serum and urine, [34] and, in the absence of in vivo data, suggested the implementation of a comparably stable metabolite into routine doping controls supported by in vitro simulation of the peptide's degradation. The additional target analyte was composed of nine amino acid residues (182)(183)(184)(185)(186)(187)(188)(189)(190) and added to a test method consisting of solid-phase extraction (SPE) and subsequent liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis, enabling an limit of detection (LOD) for AOD9604 of 50 pg/mL in human urine.…”

“…The simulation of the scenario confirmed the possibility and an advice on how to handle (self‐)catheterization for doping control sample collection with specific warning as to the possible contamination with glycerol was requested. Due to the fact that in the reported situation the prohibited substance entered the doping control sample ex vivo , complementary blood analyses as routinely conducted in clinical settings for example by isotope‐dilution mass spectrometric approaches using serum, could further support clearing an athlete of unwarranted allegations. In general, glycerol has been a major analytical challenge due to its high polarity/hydrophilicity.…”