Wu Xiujun, You Yang, Qu Gonglin, Ma Ran, Zhang Mingxue
Key Laboratory of Clinical Pharmacokinetic of TCM, Affiliated Hospital of Liaoning University of Traditional Chinese Medicine, Shenyang, China.
Key Laboratory of Radiation Protection and Nuclear Emergency of CDC, National Institute for Radiological Protection, China CDC, Beijing, China.
Biomed Chromatogr. 2017 Dec;31(12). doi: 10.1002/bmc.4019. Epub 2017 Jul 26.
A simple and sensitive HPLC-MS/MS method was developed and fully validated for simultaneous determination of ginsenoside Rb1, ginsenoside Rg1, paeoniflorin, albiflorin and oxypaeoniflorin in rat plasma. Plasma samples were pretreated with protein precipitation using acetonitrile. The chromatographic separation was carried out on a C column with a gradient mobile phase consisting of acetonitrile and water (containing 0.1% formic acid). All analytes and digoxin (internal stand, IS) were quantitated through electrospray ionization in negative ion multiple reaction monitoring mode. All calibration curves exhibited good linearity (r > 0.9960) over a wide concentration range for all components. The intra-day and inter-day precisions (RSD) at three different levels were all <12.0% and the accuracies (RE) ranging from -6.1 to 6.2%. The extraction recoveries of the five compounds ranged from 89.2 to 97.1%. The validated method was successfully applied in a comparative pharmacokinetic study of Wen-Yang-Huo-Xue soft capsule (WYHXSC) in rats. Compared with single pure component, the exposure of the investigated components, except for oxypaeoniflorin, increased after oral administration of WYHXSC in rats, which suggested a synergistic effects between the herbs in the WYHXSC preparations.
建立了一种简单灵敏的HPLC-MS/MS方法,并对其进行了全面验证,用于同时测定大鼠血浆中人参皂苷Rb1、人参皂苷Rg1、芍药苷、白芍苷和氧化芍药苷。血浆样品用乙腈进行蛋白沉淀预处理。色谱分离在C柱上进行,流动相为乙腈和水(含0.1%甲酸)的梯度洗脱。所有分析物和地高辛(内标,IS)通过电喷雾电离在负离子多反应监测模式下进行定量。所有校准曲线在各组分的宽浓度范围内均表现出良好的线性(r > 0.9960)。三种不同浓度水平的日内和日间精密度(RSD)均<12.0%,准确度(RE)在-6.1%至6.2%之间。五种化合物的提取回收率在89.2%至97.1%之间。该验证方法成功应用于大鼠温阳活血软胶囊(WYHXSC)的比较药代动力学研究。与单一纯组分相比,大鼠口服WYHXSC后,除氧化芍药苷外,所研究组分的暴露量增加,这表明WYHXSC制剂中各草药之间存在协同作用。