title: Ultra-high-performance liquid chromatography tandem mass spectrometry method for the determination of gambogenic acid in dog plasma and its application to a pharmacokinetic study.
abstract: A highly sensitive and rapid ultra-high-performance liquid chromatography-tandem mass spectrometry method was developed and validated for the determination of gambogenic acid in dog plasma. Gambogic acid was used as an internal standard (IS). After a simple liquid-liquid extraction by ethyl acetate, the analyte and internal standard were separated on an Acquity BEH C18 (100 × 2.1 mm, 1.7 µm; Waters ) column at a flow rate of 0.2 mL/min, using 0.1% formic acid-methanol (10:90, v/v) as mobile phase. Electrospray ionization source was applied and operated in the positive ion mode. Multiple reaction monitoring mode with the transitions m/z 631.3 → 507.3 and m/z 629.1 → 573.2 was used to quantify gambogenic acid and the internal standard, respectively. The calibration curves were linear in the range of 5-1000 ng/mL, with a coefficient of determination (r) of 0.999 and good calculated accuracy and precision. The low limit of quantification was 5 ng/mL. The intra-and inter-day precisions (relative standard deviations) were <15%. The methodology recoveries were more than 66.63%. This validated method was successfully applied to a pharmacokinetic study after intravenous injection administration of gambogenic acid in dogs at a dose of 1 mg/kg.
authors.affiliation: College of Pharmacy, Laboratory of Drug Metabolism and Pharmacokinetics, Anhui University of Chinese Medicine, Hefei, Anhui, China.
authors.forename: Jin Pei
authors.initials: JP
authors.lastname: Chen
authors.forename: Dian Lei
authors.initials: DL
authors.lastname: Wang
authors.forename: Li Li
authors.initials: LL
authors.lastname: Yang
authors.forename: Chen Yin
authors.initials: CY
authors.lastname: Wang
authors.forename: Shan Shan
authors.initials: SS
authors.lastname: Wang
mesh_terms: D061605:Administration, Intravenous; D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004285:Dogs; D004355:Drug Stability; D016014:Linear Models; D008297:Male; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014966:Xanthenes / Q000008:administration & dosage / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics*
chemical_list: D014966:Xanthenes; C045863:neo-gambogic acid
keywords: UHPLC-MS/MS; dog plasma; gambogenic acid; pharmacokinetics