Determination of silodosin in human plasma by liquid chromatography-tandem mass spectrometry.
A rapid, sensitive and specific liquid chromatography-tandem mass spectrometric (LC-MS/MS) method has been developed and validated for the determination of silodosin in human plasma. Silodosin and internal standard (IS) were extracted from human plasma by liquid-liquid extraction using methyl t-butyl ether and analyzed on an Agilent C(8) column with the mobile phase of acetonitrile-10 mM ammonium acetate (40:60, v/v) adjusted to pH 4.5 with acetic acid. Detection was carried out by MS/MS using TurboIonSpray (TIS) ionization and multiple reaction monitoring (MRM) in the positive-ion mode. The mass transitions monitored were m/z 496.3-->261.4 and m/z 440.4-->259.3 for silodosin and IS, respectively. The standard curve was linear in the range of 0.50-50.0 ng/ml with intra- and inter-day precision of 3.2-7.2% and 2.0-7.5%, respectively. The lower limit of quantification (LLOQ) for silodosin was 0.50 ng/ml using 500 microl plasma sample. This method was successfully applied to the pharmacokinetic study in healthy volunteers.
Department of Pharmacy, Peking University First Hospital, Beijing 100034, PR China.
Xia
X
Zhao
Yuwang
Y
Liu
Junyu
J
Xu
Dan
D
Zhang
Ying
Y
Zhou
Jingkai
J
Gu
Yimin
Y
Cui
D058668:Adrenergic alpha-1 Receptor Antagonists; D002853:Chromatography, Liquid / Q000379:methods*; D006801:Humans; D007211:Indoles / Q000097:blood* / Q000493:pharmacokinetics; D018340:Receptors, Adrenergic, alpha-1; D015203:Reproducibility of Results; D053719:Tandem Mass Spectrometry / Q000379:methods*
C547713:ADRA1A protein, human; D058668:Adrenergic alpha-1 Receptor Antagonists; D007211:Indoles; D018340:Receptors, Adrenergic, alpha-1; C095285:silodosin