Du Peng, Lei Mingdao, Liu Yu, Yang Shilin
College of Pharmacy, Soochow University, Suzhou 215123, China.
Drug Clinical Trial Institution, the Affiliated Hospital of Guizhou Medical University, Guiyang 550004, China.
Int J Mol Sci. 2016 Dec 28;18(1):45. doi: 10.3390/ijms18010045.
A specific and reliable HPLC-MS/MS method was developed and validated for the simultaneous determination of protocatechuic acid (PCA), scopolin, (-)-pinoresinol-4,4'-di--β-d-glucopyranoside (PDG), acanthoside D, acanthoside B and hyperin in rat plasma for the first time. The analytes were separated on a C column (50 × 2.1 mm, 1.8 µm) and a triple-quadrupole mass spectrometer equipped with an electrospray ionization (ESI) source was used for detection. The rat plasma sample was prepared using the protein precipitation procedure. The calibration curves were linear over a concentration range of 1.2-1200.0 ng/mL for PCA, 0.96-960.0 ng/mL for scopolin, 1.12-1120.0 ng/mL for PDG, 1.32-1320.0 ng/mL for acanthoside D, 0.99-990.0 ng/mL for acanthoside B and 1.01-1010.0 ng/mL for hyperin. The intra-day and inter-day precision was less than 11.4% and the relative error (RE) was all within ±15%. The validated method was successfully applied to assess the pharmacokinetics characteristics after the extracts of fruits were orally administered to the Sprague-Dawley rat.
首次建立并验证了一种特异性强且可靠的HPLC-MS/MS方法，用于同时测定大鼠血浆中原儿茶酸（PCA）、东莨菪苷、（-）-松脂醇-4,4'-二-β-D-吡喃葡萄糖苷（PDG）、刺五加苷D、刺五加苷B和金丝桃苷。分析物在C柱（50×2.1mm，1.8μm）上分离，采用配备电喷雾电离（ESI）源的三重四极杆质谱仪进行检测。大鼠血浆样品采用蛋白沉淀法制备。PCA的校准曲线在1.2 - 1200.0 ng/mL浓度范围内呈线性，东莨菪苷为0.96 - 960.0 ng/mL，PDG为1.12 - 1120.0 ng/mL，刺五加苷D为1.32 - 1320.0 ng/mL，刺五加苷B为0.99 - 990.0 ng/mL，金丝桃苷为1.01 - 1010.0 ng/mL。日内和日间精密度均小于11.4%，相对误差（RE）均在±15%以内。该验证方法成功应用于评估将果实提取物口服给予Sprague-Dawley大鼠后的药代动力学特征。
