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Qualitative detection of desmopressin in plasma by liquid chromatography-tandem mass spectrometry

Simone Esposito (UGent), Koen Deventer (UGent), Guy T'Sjoen (UGent), Anna Vantilborgh (UGent), Frans Delbeke (UGent), An-Sofie Goessaert (UGent), Karel Everaert (UGent) and Peter Van Eenoo (UGent)
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Abstract
This work describes a liquid chromatography-electrospray tandem mass spectrometry method for detection of desmopressin in human plasma in the low femtomolar range. Desmopressin is a synthetic analogue of the antidiuretic hormone arginine vasopressin and it might be used by athletes as a masking agent in the framework of blood passport controls. Therefore, it was recently added by the World Anti-Doping Agency to the list of prohibited substances in sport as a masking agent. Mass spectrometry characterization of desmopressin was performed with a high-resolution Orbitrap-based mass spectrometer. Detection of the peptide in the biological matrix was achieved using a triple-quadrupole instrument with an electrospray ionization interface after protein precipitation, weak cation solid-phase extraction and high performance liquid chromatography separation with an octadecyl reverse-phase column. Identification of desmopressin was performed using three product ions, m/z 328.0, m/z 120.0, and m/z 214.0, from the parent ion, m/z 535.5. The extraction efficiency of the method at the limit of detection was estimated as 40% (n = 10), the ion suppression as 5% (n = 10), and the limit of detection was 50 pg/ml (signal-to-noise ratio greater than 3). The selectivity of the method was verified against several endogenous and synthetic desmopressin-related peptides. The performance and the applicability of the method were tested by analysis of clinical samples after administration of desmopressin via intravenous, oral, and intranasal routes. Only after intravenous administration could desmopressin be successfully detected.
Keywords
EXCRETION, PHARMACOKINETICS, DIABETES-INSIPIDUS, NOCTURNAL POLYURIA, 1-DEAMINO-8-D-ARGININE VASOPRESSIN, Plasma, Doping, Desmopressin, Liquid chromatography-mass spectrometry, ADULTS

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Citation

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Chicago
Esposito, Simone, Koen Deventer, Guy T’Sjoen, Anna Vantilborgh, Frans Delbeke, An-Sofie Goessaert, Karel Everaert, and Peter Van Eenoo. 2012. “Qualitative Detection of Desmopressin in Plasma by Liquid Chromatography-tandem Mass Spectrometry.” Analytical and Bioanalytical Chemistry 402 (9): 2789–2796.
APA
Esposito, S., Deventer, K., T’Sjoen, G., Vantilborgh, A., Delbeke, F., Goessaert, A.-S., Everaert, K., et al. (2012). Qualitative detection of desmopressin in plasma by liquid chromatography-tandem mass spectrometry. ANALYTICAL AND BIOANALYTICAL CHEMISTRY, 402(9), 2789–2796.
Vancouver
1.
Esposito S, Deventer K, T’Sjoen G, Vantilborgh A, Delbeke F, Goessaert A-S, et al. Qualitative detection of desmopressin in plasma by liquid chromatography-tandem mass spectrometry. ANALYTICAL AND BIOANALYTICAL CHEMISTRY. 2012;402(9):2789–96.
MLA
Esposito, Simone, Koen Deventer, Guy T’Sjoen, et al. “Qualitative Detection of Desmopressin in Plasma by Liquid Chromatography-tandem Mass Spectrometry.” ANALYTICAL AND BIOANALYTICAL CHEMISTRY 402.9 (2012): 2789–2796. Print.
@article{3092539,
  abstract     = {This work describes a liquid chromatography-electrospray tandem mass spectrometry method for detection of desmopressin in human plasma in the low femtomolar range. Desmopressin is a synthetic analogue of the antidiuretic hormone arginine vasopressin and it might be used by athletes as a masking agent in the framework of blood passport controls. Therefore, it was recently added by the World Anti-Doping Agency to the list of prohibited substances in sport as a masking agent. Mass spectrometry characterization of desmopressin was performed with a high-resolution Orbitrap-based mass spectrometer. Detection of the peptide in the biological matrix was achieved using a triple-quadrupole instrument with an electrospray ionization interface after protein precipitation, weak cation solid-phase extraction and high performance liquid chromatography separation with an octadecyl reverse-phase column. Identification of desmopressin was performed using three product ions, m/z 328.0, m/z 120.0, and m/z 214.0, from the parent ion, m/z 535.5. The extraction efficiency of the method at the limit of detection was estimated as 40\% (n = 10), the ion suppression as 5\% (n = 10), and the limit of detection was 50 pg/ml (signal-to-noise ratio greater than 3). The selectivity of the method was verified against several endogenous and synthetic desmopressin-related peptides. The performance and the applicability of the method were tested by analysis of clinical samples after administration of desmopressin via intravenous, oral, and intranasal routes. Only after intravenous administration could desmopressin be successfully detected.},
  author       = {Esposito, Simone and Deventer, Koen and T'Sjoen, Guy and Vantilborgh, Anna and Delbeke, Frans and Goessaert, An-Sofie and Everaert, Karel and Van Eenoo, Peter},
  issn         = {1618-2642},
  journal      = {ANALYTICAL AND BIOANALYTICAL CHEMISTRY},
  keyword      = {EXCRETION,PHARMACOKINETICS,DIABETES-INSIPIDUS,NOCTURNAL POLYURIA,1-DEAMINO-8-D-ARGININE VASOPRESSIN,Plasma,Doping,Desmopressin,Liquid chromatography-mass spectrometry,ADULTS},
  language     = {eng},
  number       = {9},
  pages        = {2789--2796},
  title        = {Qualitative detection of desmopressin in plasma by liquid chromatography-tandem mass spectrometry},
  url          = {http://dx.doi.org/10.1007/s00216-011-5697-5},
  volume       = {402},
  year         = {2012},
}

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