title: Development and validation of a quantitative liquid chromatography tandem mass spectrometry assay for pristimerin in rat plasma.
abstract: A sensitive, rapid and simple LC-MS/MS analysis method was developed and validated for the determination of pristimerin (PR) in rat plasma. Protein precipitation with four volumes of acetonitrile as the precipitation reagent was used as the sample preparation method. The analysis process was performed on a Merck ZIC-HILIC column with the mobile phase of acetonitrile-water (containing 5mM ammonium formate, pH 2.8) (85:15, v/v). PR (m/z 465.3-201.1) and glycyrrhetinic acid (internal standard, m/z 471.5-177.1) were monitored under positive electrospray ionization in multiple reaction monitoring (MRM) mode. Retention time of PR and IS was 2.45min and 2.4min, respectively. The limit of detection was 0.5ng/mL and the linear range was 1-500ng/mL. The intra-day and inter-day precision were 2.89-6.27% and 4.91-8.98%, and the intra-day and inter-day accuracy ranged from -5.81% to 8.64% and -7.37% to 9.57%, respectively. The matrix effects and absolute recovery ranged from 89.3% to 92.4% and 88.7% to 92.8%, respectively. The method has been successfully applied to the determination of PR concentration in rat plasma after intravenous administration (0.5mg/kg).
authors.affiliation: Department of Pharmacology, Institute of Medical Sciences, Shanghai Jiao Tong University School of Medicine, 280 South Chongqing Road, Shanghai 200025, China.
authors.forename: Xin
authors.initials: X
authors.lastname: Luan
authors.forename: Ying-Yun
authors.initials: YY
authors.lastname: Guan
authors.forename: Ya-Rong
authors.initials: YR
authors.lastname: Liu
authors.forename: Chao
authors.initials: C
authors.lastname: Wang
authors.forename: Mei
authors.initials: M
authors.lastname: Zhao
authors.forename: Qin
authors.initials: Q
authors.lastname: Lu
authors.forename: Ya-Bin
authors.initials: YB
authors.lastname: Tang
authors.forename: Xiao-Lin
authors.initials: XL
authors.lastname: Wang
authors.forename: Chao
authors.initials: C
authors.lastname: Fang
authors.forename: Hong-Zhuan
authors.initials: HZ
authors.lastname: Chen
mesh_terms: D000818:Animals; D002853:Chromatography, Liquid / Q000379:methods*; D005260:Female; D053978:Pentacyclic Triterpenes; D051381:Rats; D017207:Rats, Sprague-Dawley; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014315:Triterpenes / Q000097:blood* / Q000493:pharmacokinetics
chemical_list: D053978:Pentacyclic Triterpenes; D014315:Triterpenes; C050414:celastrol
keywords: HPLC–MS/MS; Pharmacokinetics; Pristimerin; Rat plasma