title: Simultaneous determination of udenafil and its active metabolite, DA-8164, in human plasma and urine using ultra-performance liquid chromatography-tandem mass spectrometry: application to a pharmacokinetic study.
abstract: A rapid, sensitive, and simple ultra-performance liquid chromatography-tandem mass spectrometry (UPLC/MS/MS) method for the determination of udenafil and its active metabolite, DA-8164, in human plasma and urine using sildenafil as an internal standard (IS) was developed and validated. Udenafil, DA-8164 and IS from a 100 microL aliquot of biological samples were extracted by protein precipitation using acetonitrile. Chromatographic separation was carried on an Acquity UPLC BEH C(18) column (50 x 2.1 mm, i.d., 1.7 microm) with an isocratic mobile phase consisting of acetonitrile and containing 0.1% formic acid (75:25, v/v) at flow rate of 0.4 mL/min, and total run time was within 1 min. Detection and quantification was performed by the mass spectrometer using multiple reaction-monitoring mode at m/z 517 --> 283 for udenafil, m/z 406 --> 364 for DA-8164 and m/z 475 --> 100 for IS. The assay was linear over a concentration range of 1-600 ng/mL with a lower limit of quantification of 1 ng/mL in both human plasma and urine. The coefficient of variation of this assay precision was less than 13.7%, and the accuracy exceeded 92.0%. This method was successfully applied for pharmacokinetic study after oral administration of udenafil 100 mg to healthy Korean male volunteers.
authors.affiliation: Department of Clinical Pharmacology and Clinical Trial Center, Inje University Busan Paik Hospital, Busan, Korea.
authors.forename: Soo Kyung
authors.initials: SK
authors.lastname: Bae
authors.forename: Min Jeong
authors.initials: MJ
authors.lastname: Kang
authors.forename: Chang-Woo
authors.initials: CW
authors.lastname: Yeo
authors.forename: Min-Jung
authors.initials: MJ
authors.lastname: Kim
authors.forename: Ji-Hong
authors.initials: JH
authors.lastname: Shon
authors.forename: Kwang-Hyeon
authors.initials: KH
authors.lastname: Liu
authors.forename: Jae-Gook
authors.initials: JG
authors.lastname: Shin
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D006801:Humans; D008297:Male; D011743:Pyrimidines / Q000097:blood / Q000493:pharmacokinetics* / Q000652:urine; D012680:Sensitivity and Specificity; D013449:Sulfonamides; D053719:Tandem Mass Spectrometry / Q000379:methods*; D000096926:Benzenesulfonamides
chemical_list: D011743:Pyrimidines; D013449:Sulfonamides; C502127:DA-8164; C419664:udenafil; D000096926:Benzenesulfonamides