School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China; State Key Laboratory of Drug Delivery Technology and Pharmacokinetics, Tianjin Institute of Pharmaceutical Research, Tianjin 300193, China.
State Key Laboratory of Drug Delivery Technology and Pharmacokinetics, Tianjin Institute of Pharmaceutical Research, Tianjin 300193, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Aug 1;1091:29-35. doi: 10.1016/j.jchromb.2018.05.020. Epub 2018 May 20.
A simple, sensitive and selective LC-MS/MS method was developed for the quantitative analysis of liraglutide and validated in rat plasma. Human insulin was used as the internal standard. After a simple protein precipitation step, liraglutide was chromatographically separated using an InertSustain Bio C18 column with mobile phases comprising acetonitrile with 0.1% formic acid (A) and water with 0.1% formic acid (B). Detection was achieved using positive ion electrospray ionization in multiple-reaction monitoring (MRM) mode. Good linearity was observed in the concentration range 0.5-250 ng/mL (r > 0.99). The intra- and inter-day precision values (expressed as relative standard deviation, RSD) of liraglutide ranged from 1.97-7.63% and 5.25-11.9, respectively. The accuracy (expressed as relative error, RE) ranged from -8.79-11.4%. Both the recovery and matrix effect were within acceptable limits. This method was successfully applied for the pharmacokinetics study of liraglutide in rats after subcutaneous administration.
建立了一种简单、灵敏、选择性的 LC-MS/MS 法，用于定量分析利拉鲁肽，并在大鼠血浆中进行了验证。人胰岛素被用作内标。在简单的蛋白沉淀步骤后，利拉鲁肽采用 InertSustain Bio C18 柱进行色谱分离，流动相由含 0.1%甲酸的乙腈（A）和含 0.1%甲酸的水（B）组成。采用正离子电喷雾电离，在多重反应监测（MRM）模式下进行检测。在 0.5-250ng/mL 的浓度范围内，观察到良好的线性（r>0.99）。利拉鲁肽的日内和日间精密度（表示为相对标准偏差，RSD）分别在 1.97-7.63%和 5.25-11.9 之间。准确度（表示为相对误差，RE）在-8.79-11.4%之间。回收率和基质效应均在可接受范围内。该方法成功应用于皮下给予利拉鲁肽后大鼠的药代动力学研究。
