Validated UPLC-MS/MS method for the determination of tadalafil in human plasma and its application to a pharmacokinetic study.
10.12793/tcp.2017.25.1.21
- Author:
Kwang Youl KIM
1
;
Moonsuk NAM
;
Hyun Jung KWON
;
Kwang Hyeon KIM
;
Seung Hyun KANG
;
Sang Il KIM
;
Cheol Woo KIM
;
Sang Heon CHO
Author Information
1. Department of Clinical Pharmacology, Inha University Hospital, Inha University School of Medicine, Incheon 22332, South Korea. shcho123@inha.ac.kr
- Publication Type:Original Article
- Keywords:
Tadalafil;
Pharmacokinetics;
UPLC;
Plasma
- MeSH:
Ammonium Compounds;
Humans*;
Male;
Methods*;
Pharmacokinetics;
Plasma*;
Sildenafil Citrate;
Tadalafil*
- From:Translational and Clinical Pharmacology
2017;25(1):21-27
- CountryRepublic of Korea
- Language:English
-
Abstract:
A simple, rapid, and reliable UPLC-MS/MS method was developed and validated for the determination of tadalafil in human plasma. The plasma samples were deproteinized with acetonitrile. Chromatographic separation was performed on a Shiseido C18 (100 × 2.1 mm, 2.7 µm) column with isocratic elution using 2.0 mM ammonium acetate and acetonitrile (55:45, v/v) with 0.1% formic acid at a flow rate of 0.7 mL/min. The total run time was 1 min per sample. The quantitative analysis was performed using multiple reaction monitoring at transition of m/z 390.4 → 268.3 for tadalafil and m/z 475.3 → 283.3 for sildenafil as an internal standard. The method was fully validated over a concentration range of 5–1,000 ng/mL with a lower quantification limit of 5 ng/mL. Intra- and inter-day precision (relative standard deviation, %RSD) were within 8.4% and accuracy (relative error, %RE) was lower than -3.2%. The developed and validated method was successfully applied to a pharmacokinetic study of tadalafil (20 mg) in Korean healthy male subjects (n = 12).