Doping control analysis of desmopressin in human urine by LC-ESI-MS/MS after urine delipidation

作者：Esposito Simone^*; Deventer Koen; T' Sjoen Guy; Vantilborgh Anna; Van Eenoo Peter

来源：Biomedical Chromatography, 2013, 27(2): 240-245.

DOI：10.1002/bmc.2782

• desmopressin
• LC-MS
• doping
• urine
• delipidation

The World Anti-Doping Agency (WADA) has recently added desmopressin, a synthetic analogue of the endogenous peptide hormone arginine vasopressin, to the Prohibited List, owing to the potential masking effects of this drug on hematic parameters useful to detect blood doping. A qualitative method for detection of desmopressin in human urine by high-performance liquid chromatographyelectrospray tandem mass spectrometry (LC-ESI-MS/MS) has been developed and validated. Desmopressin purification from urine was achieved by means of delipidation with a 60:40 di-isopropyl ether/n-butanol and solid-phase extraction with WCX cartridges. The lower limit of detection was 25?pg/mL. Extraction recovery was determined as 59.3% (SD 29.4), and signal reduction owing to ion suppression was estimated to be 42.7% (SD 12.9). The applicability of the method was proven by the analysis of real urine samples obtained after intravenous, oral and intranasal administration of desmopressin, achieving unambiguous detection of the peptide in all the cases.

• 出版日期2013-2