Yin Xingbin, Lin Longfei, Shen Mingrui, Zhai Yujing, Cao Sali, Fu Jing, Li Xuechun, Yang Chunjing, Xia Zhenwen, Zhao Yang, Li Shangxin, Bai Ying, Xue Dan, Ni Jian
School of Chinese Materia Medica, Beijing University of Chinese Medicine, Beijing, 100102, China.
Biomed Chromatogr. 2014 Dec;28(12):1869-73. doi: 10.1002/bmc.3236. Epub 2014 Jun 5.
A highly sensitive, rapid assay method has been developed and validated for the analysis of polyphyllin H in beagle dog plasma with liquid chromatography coupled to tandem mass spectrometry with electrospray ionization in the positive-ion mode. The assay procedure involves extraction of polyphyllin H and ginsenoside Re (IS) from beagle dog plasma. Chromatographic separation was carried out on an Agilent Zorbax XDB-C18 (100 × 2.1 mm, 1.8μm) column by isocratic elution with acetonitrile and water (50:50, v/v) at a flow rate of 0.25 mL/min with a total run time of 2.5 min. The MS/MS ion transitions monitored were m/z 869.60 → 869.60 for polyphyllin H and m/z 969.60 → 969.60 for IS. [corrected] Linear responses were obtained for polyphyllin H ranging from 1 to 50 ng/mL. The intra-and inter-day precisions (RSDs) <1.77 and 3.39% and the extraction recovery ranged from 91.89 to 93.33% with RSD <2.68%. Stability studies showed that polyphyllin H was stable in the preparation and analytical process. The results indicated that the validated method was successfully used to determine the concentration-time profiles of polyphyllin H.
已开发并验证了一种高灵敏度、快速的分析方法，用于采用液相色谱-串联质谱联用（正离子模式下的电喷雾电离）分析比格犬血浆中的重楼皂苷H。该分析方法包括从比格犬血浆中提取重楼皂苷H和人参皂苷Re（内标）。色谱分离在Agilent Zorbax XDB-C18（100×2.1 mm，1.8μm）柱上进行，采用乙腈和水（50:50，v/v）等度洗脱，流速为0.25 mL/min，总运行时间为2.5分钟。监测的MS/MS离子跃迁为：重楼皂苷H的m/z 869.60→869.60，内标的m/z 969.60→969.60。重楼皂苷H在1至50 ng/mL范围内获得线性响应。日内和日间精密度（RSD）分别<1.77%和3.39%，提取回收率在91.89%至93.33%之间，RSD<2.68%。稳定性研究表明，重楼皂苷H在制备和分析过程中稳定。结果表明，该验证方法成功用于测定重楼皂苷H的浓度-时间曲线。
