School of Pharmaceutical Sciences, Shandong University, Wenhuaxi Road 44, Jinan 250012, Shandong Province, P.R. China.
National Glycoengineering Research Center, Shandong University, Wenhuaxi Road 44, Jinan 250012, Shandong Province, P.R. China.
J Chromatogr Sci. 2022 Feb 16;60(2):186-193. doi: 10.1093/chromsci/bmab058.
Qilong capsule (QLC) is a well-known Traditional Chinese Medicine, and it has a long history for the treatment of ischemic stroke. Its major ingredients are saponins, such as paeoniflorin, amygdalin and calycosin-7-glucoside, contributing to vasodilation function. In this study, a simple, rapid and sensitive high-performance liquid chromatography-tandem mass spectrometry method was developed to determine three bioactive ingredients in rat plasma after oral administration of QLC. A simple acetonitrile precipitation method was introduced during the sample preparation. Chromatographic separation was performed on a Shiseido CAPCELL PAC MGIII-C18 column using a gradient elution with acetonitrile and water (0.1% formic acid) as a mobile phase, and the chromatographic separation was 5 min. The methodological evaluation showed that this method had a high sensitivity (the lower limit of quantification was 1 ng/mL for calycosin-7-glucoside, 5 ng/mL for paeoniflorin, 5 ng/mL for amygdalin), satisfactory accuracy (relative error ≤ ±15%) and precision (relative standard deviation ≤15%). Then, the analytical method was applied to the pharmacokinetic study in rats following oral administration of the extracts in QLC. Meanwhile, the pharmacokinetic parameters of complex system in QLC were analyzed and the potential interaction between ingredients was explored. The present quantification method and pharmacokinetic study will provide a meaningful reference for the formulas research of QLC in the treatment of ischemic stroke.
芪龙胶囊(QLC)是一种著名的中药,用于治疗缺血性中风已有很长的历史。其主要成分是皂苷,如芍药苷、苦杏仁苷和毛蕊异黄酮苷,具有舒张血管功能。本研究建立了一种简单、快速、灵敏的高效液相色谱-串联质谱法,用于测定大鼠灌胃芪龙胶囊后血浆中的三种生物活性成分。在样品制备过程中采用了简单的乙腈沉淀法。采用 Shiseido CAPCELL PAC MGIII-C18 柱,以乙腈和水(0.1%甲酸)为流动相进行梯度洗脱,色谱分离在 5 min 内完成。方法学评价表明,该方法具有高灵敏度(毛蕊异黄酮苷的定量下限为 1 ng/mL,芍药苷和苦杏仁苷的定量下限为 5 ng/mL)、良好的准确性(相对误差≤±15%)和精密度(相对标准偏差≤15%)。然后,该分析方法应用于大鼠灌胃 QLC 提取物后的药代动力学研究。同时,分析了 QLC 中复杂体系的药代动力学参数,并探讨了成分之间的潜在相互作用。本定量方法和药代动力学研究将为 QLC 治疗缺血性中风的配方研究提供有意义的参考。