title: Development and validation of an LC-MS/MS method for the determination of pelubiprofen and its active metabolite, trans-alcohol, in human plasma and its application to pharmacokinetic study.
abstract: A suitable liquid chromatography tandem mass spectrometry (LC-MS/MS) method is required to determine pelubiprofen and its active metabolite, trans-alcohol (M-D), in human plasma for pharmacokinetic studies of pelubiprofen preparations. After one-step liquid-liquid extraction (LLE) using methyl tert-butyl ether (MTBE), pelubiprofen, M-D, and tolbutamide (the internal standard, IS) were eluted from a Capcellpak C18 ACR column using a gradient mobile phase consisting of 0.1% formic acid in water and acetonitrile at a flow rate 0.35mL/min. The achieved lower limits of quantitation (LLOQ) of pelubiprofen and M-D were both 15ng/mL (S/N>10) and the standard calibration curves for pelubiprofen and M-D were linear (correlation coefficients >0.99) over the studied concentration range (15-2000ng/mL). Intra- and inter-day precisions were within 7.62% for all analytes and the deviation of assay accuracies was within ±13.23%. The developed method was successfully applied to a pharmacokinetic study of pelubiprofen in healthy Korean male volunteers.
authors.affiliation: Department of Pharmaceutical Biochemistry, Medical Center, Kyung Hee University, Hoegi-Dong, Dongdaemun-gu, Seoul, 130-701, Republic of Korea; Department of Life and Nanopharmaceutical Science, and Medical Center, Kyung Hee University, Hoegi-Dong, Dongdaemun-gu, Seoul, 130-701, Republic of Korea.
authors.forename: Ju-Hee
authors.initials: JH
authors.lastname: Ryu
authors.affiliation: Kyung Hee Drug Analysis Center, College of Pharmacy, Medical Center, Kyung Hee University, Hoegi-Dong, Dongdaemun-gu, Seoul, 130-701, Republic of Korea.
authors.forename: Ji-Sun
authors.initials: JS
authors.lastname: Park
authors.affiliation: Department of Pharmaceutical Biochemistry, Medical Center, Kyung Hee University, Hoegi-Dong, Dongdaemun-gu, Seoul, 130-701, Republic of Korea.
authors.forename: Min-Ho
authors.initials: MH
authors.lastname: Jo
authors.affiliation: Department of Pharmaceutical Biochemistry, Medical Center, Kyung Hee University, Hoegi-Dong, Dongdaemun-gu, Seoul, 130-701, Republic of Korea; Daewon Pharm Co., Ltd, 389 Chenhodaero, Kwangjin-ku, Seoul 467-24, Republic of Korea.
authors.forename: Joo-Il
authors.initials: JI
authors.lastname: Kim
authors.affiliation: Kyung Hee Drug Analysis Center, College of Pharmacy, Medical Center, Kyung Hee University, Hoegi-Dong, Dongdaemun-gu, Seoul, 130-701, Republic of Korea.
authors.forename: Wang-Seob
authors.initials: WS
authors.lastname: Shim
authors.affiliation: Medical Center, Kyung Hee University, Hoegi-Dong, Dongdaemun-gu, Seoul, 130-701, Republic of Korea.
authors.forename: Bo-Hyung
authors.initials: BH
authors.lastname: Kim
authors.affiliation: Medical Center, Kyung Hee University, Hoegi-Dong, Dongdaemun-gu, Seoul, 130-701, Republic of Korea.
authors.forename: Sung-Vin
authors.initials: SV
authors.lastname: Yim
authors.affiliation: Department of Life and Nanopharmaceutical Science, and Medical Center, Kyung Hee University, Hoegi-Dong, Dongdaemun-gu, Seoul, 130-701, Republic of Korea.
authors.forename: Jongki
authors.initials: J
authors.lastname: Hong
authors.affiliation: Department of Pharmaceutical Biochemistry, Medical Center, Kyung Hee University, Hoegi-Dong, Dongdaemun-gu, Seoul, 130-701, Republic of Korea; Department of Life and Nanopharmaceutical Science, and Medical Center, Kyung Hee University, Hoegi-Dong, Dongdaemun-gu, Seoul, 130-701, Republic of Korea; Kyung Hee Drug Analysis Center, College of Pharmacy, Medical Center, Kyung Hee University, Hoegi-Dong, Dongdaemun-gu, Seoul, 130-701, Republic of Korea. Electronic address: ktlee@khu.ac.kr.
authors.forename: Kyung-Tae
authors.initials: KT
authors.lastname: Lee
mesh_terms: D000328:Adult; D000438:Alcohols / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics*; D002853:Chromatography, Liquid / Q000379:methods*; D006801:Humans; D057230:Limit of Detection; D008297:Male; D010666:Phenylpropionates / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics*; D012015:Reference Standards; D015203:Reproducibility of Results; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014044:Tolbutamide / Q000737:chemistry
chemical_list: C000602097:2-(4-((2-hydroxycyclohexylidene)methyl)phenyl)propionic acid; D000438:Alcohols; D010666:Phenylpropionates; C040375:pelubiprofen; D014044:Tolbutamide
keywords: Human plasma; LC-MS/MS; Liquid–liquid extraction; Metabolite; Pelubiprofen; Pharmacokinetic study