title: Determination of Pseudoginsengenin DQ in rat plasma by UPLC-MS/MS and application of the method in a pharmacokinetic study.
abstract: Pseudoginsengenin DQ (pseudoginsengenin of diol derivatives quest, PDQ), the product of the oxidative cyclization of protopanaxadiol, exhibits a significant pharmacological effect as an antiarrhythmic agent. A sensitive and rapid analytical method based on ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) was initially developed for the detection of PDQ in rat plasma. Pre-treatment of the sample obtained from the plasma involved a single protein precipitation step, using methanol. PDQ and an internal standard (IS), physcion, were separated on a Waters ACQUITY UPLC BEH C18 analytical column (50mm×2.1mm, 1.7μm) using acetonitrile-0.1% formic acid in water (70:30, v/v) as the mobile phase, at a flow rate of 0.3mL/min. Chromatography of the PDQ and IS was performed within 3min. Detection was performed through positive ion electrospray ionization (ESI(+)) in multiple reaction-monitoring (MRM) mode. The assay was linear over the concentration range of 5-1000ng/mL (r>0.9980). The limit of detection (LOD) and the lower limit of quantification (LLOQ) were 0.5ng/mL and 5.0ng/mL, respectively. The intra- and inter-day deviations (expressed as relative standard deviation, RSD) were ≤9.5% and ≤1.7%, respectively, and the accuracy (expressed as relative error, RE) was in the range of -1.1 to 2.7%. The recoveries of PDQ and IS were 95.2% and 100.7%, respectively, and the matrix effects were satisfactory in all of the biological matrices examined. This fully validated method was successfully applied to the pharmacokinetic study of rats after a single initial intragastric administration of 15mg/kg PDQ. The main pharmacokinetic parameters: Tmax (the time to peak), Cmax (the concentration to peak), and t1/2 (the biological half time) were 4.0±0.0h, 3265.12±700.26ng/mL, 5.97±0.43h, respectively.
authors.affiliation: Institute of Frontier Medical Science of Jilin University, ChangChun, Jilin 130021, China.
authors.forename: Hongmei
authors.initials: H
authors.lastname: Gao
authors.forename: Zhuo
authors.initials: Z
authors.lastname: Li
authors.forename: Pingya
authors.initials: P
authors.lastname: Li
authors.forename: Meiyu
authors.initials: M
authors.lastname: Lin
authors.forename: Liu
authors.initials: L
authors.lastname: Han
authors.forename: Fang
authors.initials: F
authors.lastname: Wang
authors.forename: Jinping
authors.initials: J
authors.lastname: Liu
mesh_terms: D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D057230:Limit of Detection; D008297:Male; D051381:Rats; D017208:Rats, Wistar; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D014315:Triterpenes / Q000097:blood* / Q000493:pharmacokinetics
chemical_list: D014315:Triterpenes
keywords: Pharmacokinetics; Pseudoginsengenin DQ; UPLC–MS/MS