title: Development of a rapid UPLC-MS/MS method for quantification of saxagliptin in rat plasma and application to pharmacokinetic study.
abstract: A novel, simple and rapid ultraperformance liquid chromatography/tandem mass spectrometry (UPLC-MS/MS) assay was established for quantification of saxagliptin in rat plasma. Plasma samples were processed by liquid-liquid extraction with ethyl acetate and chromatographed on a C₁₈ column (2.1 × 50 mm i.d., 1.7 µm). The mobile phase consisted of methanol and 0.1% formic acid (40:60, v/v). Multiple reaction monitoring transitions were performed for detection in positive-ion mode with an electrospray ionization source. The calibration curve was linear over the concentration range of 0.5-100 ng/mL (R²  > 0.99). All accuracy values were between 90.62 and 105.60% relative error and the intra- and inter-day precisions were less than 9.66% relative standard deviation. Extraction recovery was more than 81.01% and the matrix effect ranged from 90.27 to 109.15%. After validation, the method was applied to a pharmacokinetic study where healthy rats were orally given 0.5 mg/kg saxagliptin.
authors.affiliation: School of Pharmaceutical Sciences, Sun Yat-sen University, Guangzhou 510006, China.
authors.forename: Jing-wen
authors.initials: JW
authors.lastname: Gao
authors.forename: Yue-mei
authors.initials: YM
authors.lastname: Yuan
authors.forename: Ya-song
authors.initials: YS
authors.lastname: Lu
authors.forename: Mei-cun
authors.initials: MC
authors.lastname: Yao
mesh_terms: D000085:Acetates / Q000737:chemistry; D000218:Adamantane / Q000031:analogs & derivatives* / Q000097:blood / Q000737:chemistry / Q000493:pharmacokinetics; D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004151:Dipeptides / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics; D054873:Dipeptidyl-Peptidase IV Inhibitors / Q000097:blood / Q000737:chemistry / Q000493:pharmacokinetics; D004355:Drug Stability; D016018:Least-Squares Analysis; D008297:Male; D051381:Rats; D017208:Rats, Wistar; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D000085:Acetates; D004151:Dipeptides; D054873:Dipeptidyl-Peptidase IV Inhibitors; C007650:ethyl acetate; C502994:saxagliptin; D000218:Adamantane