Gao Jing-wen, Yuan Yue-mei, Lu Ya-song, Yao Mei-cun
School of Pharmaceutical Sciences, Sun Yat-sen University, Guangzhou 510006, China.
Biomed Chromatogr. 2012 Dec;26(12):1482-7. doi: 10.1002/bmc.2720. Epub 2012 Feb 15.
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.
建立了一种新颖、简单且快速的超高效液相色谱/串联质谱（UPLC-MS/MS）法，用于定量大鼠血浆中的沙格列汀。血浆样品采用乙酸乙酯液-液萃取法处理，并在C₁₈柱（内径2.1×50 mm，1.7 µm）上进行色谱分析。流动相由甲醇和0.1%甲酸（40:60，v/v）组成。采用电喷雾电离源在正离子模式下进行多反应监测转换以进行检测。校准曲线在0.5-100 ng/mL的浓度范围内呈线性（R²＞0.99）。所有准确度值的相对误差在90.62%至105.60%之间，日内和日间精密度的相对标准偏差均小于9.66%。萃取回收率超过81.01%，基质效应在90.27%至109.15%之间。经过验证后，该方法应用于一项药代动力学研究，给健康大鼠口服0.5 mg/kg沙格列汀。
