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- Title
Simultaneous quantification and qualification of synacthen in plasma.
- Authors
Chaabo, Ayman; De Ceaurriz, Jacques; Buisson, Corinne; Tabet, Jean-Claude; Lasne, Françoise
- Abstract
Tetracosactide (Synacthen), a synthetic analogue of adrenocorticotropic hormone (ACTH), can be used as a doping agent to increase the secretion of glucocorticoids by adrenal glands. The only published method for anti-doping control of this drug in plasma relies on purification by immunoaffinity chromatography and LC/MS/MS analysis. Its limit of detection is 300 pg/mL, which corresponds to the peak value observed 12 h after 1 mg Synacthen IM administration. We report here a more sensitive method based on preparation of plasma by cation exchange chromatography and solid-phase extraction and analysis by LC/MS/MS with positive-mode electrospray ionization using 7-38 ACTH as internal standard. Identification of Synacthen was performed using two product ions, m/ z 671.5 and m/ z 223.0, from the parent [M + 5H] ion, m/ z 587.4. The recovery was estimated at 70%. A linear calibration curve was obtained from 25 to 600 pg/mL ( R > 0.99). The lower limit of detection was 8 pg/mL (S/ N > 3). The lower limit of quantification was 15 pg/mL ( S/ N > 10; CV% < 20%). The performance of the method was illustrated by an 8-h kinetic analysis of plasma samples from nine subjects submitted to IM injections of either Synacthen® (five subjects) or Synacthen® Depot, the slow-release form of the drug (four subjects). Concentrations of Synacthen between 16 and 310 pg/mL were observed. A sensitive method for quantitation of Synacthen in plasma is proposed for anti-doping control analyses.
- Subjects
ADRENOCORTICAL hormones; TANDEM mass spectrometry; ADRENAL glands; CHROMATOGRAPHIC analysis; GLUCOCORTICOIDS
- Publication
Analytical & Bioanalytical Chemistry, 2011, Vol 399, Issue 5, p1835
- ISSN
1618-2642
- Publication type
Academic Journal
- DOI
10.1007/s00216-010-4565-z