Detection of budesonide in human urine after inhalation by liquid chromatography-mass spectrometry.
Budesonide, a corticosteroid frequently used in the treatment of asthma, is most often administered via inhalation. Its use in sports is allowed when medically necessary. A fast, sensitive and accurate LC-MS method was developed and validated for the quantification of budesonide and its major metabolite 16alpha-hydroxyprednisolone in urine samples after inhalation of a metered dose (Pulmicort-Turbohaler 200). Sample preparation consists of an alkaline liquid-liquid extraction with ethyl acetate. Analysis was performed using liquid chromatography-tandem mass spectrometry with electrospray ionization (ESI). The method was linear in the range of 5-100 and 0.5-10ng/mL for 16alpha-hydroxyprednisolone and budesonide, respectively. The limits of quantification were 5ng/ml for 16alpha-hydroxyprednisolone and 0.5ng/mL for budesonide. The accuracy ranged from 2.2 to 3.5% for 16alpha-hydroxyprednisolone and from 0.8 to 16.4% for budesonide. After administration of 200microg of budesonide to five healthy volunteers budesonide could not be detected in any urine sample whereas 16alpha-hydroxyprednisolone was detectable up to 12h post-administration.
Deventer
K
K
Doping Control Laboratory (DoCoLab), Ghent University, UGent, Technologiepark 30B, B-9052 Zwijnaarde, Belgium. Koen.Deventer@UGent.be
Mikulcíková
P
P
Van Hoecke
H
H
Van Eenoo
P
P
Delbeke
F T
FT
D000280:Administration, Inhalation; D000328:Adult; D000893:Anti-Inflammatory Agents / Q000008:administration & dosage / Q000737:chemistry / Q000378:metabolism / Q000652:urine*; D019819:Budesonide / Q000008:administration & dosage / Q000737:chemistry / Q000378:metabolism / Q000652:urine*; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D006801:Humans; D008297:Male; D036501:Metered Dose Inhalers; D011239:Prednisolone / Q000031:analogs & derivatives / Q000378:metabolism / Q000652:urine; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods
C093190:16-hydroxyprednisolone; D000893:Anti-Inflammatory Agents; D019819:Budesonide; D011239:Prednisolone