Yin Xingbin, Li Zhaoxia, Zhai Yujing, Zhang Hui, Lin Longfei, Yang Pei, Cao Sali, Zhang Jin, Qi Juanjuan, Tian Jingchen, Fu Jing, Qu Changhai, Ni Jian
School of Chinese Materia Medica, Beijing University of Chinese Medicine, Beijing, 100102, China.
Biomed Chromatogr. 2013 Jun;27(6):807-11. doi: 10.1002/bmc.2865. Epub 2013 Feb 7.
A highly sensitive, rapid assay method has been developed and validated for the analysis of hyperoside 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 hyperoside and ginsenoside Re (IS) from beagle dog plasma. Chromatographic separation was carried out on an Agilent Zorbax XDB-C18 (100 × 2.1 mm, 1.8 µm) 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 2.0 min. The MS/MS ion transitions monitored were 464.4 → 463.4 for hyperoside and 947.12 → 969.60 for IS. Linear responses were obtained for hyperoside ranging from 10 to 5000 ng/mL. The intra-and inter-day precisions (RSDs) were <5.38 and 3.39% and the extraction recovery ranged from 94.39 to 100.78% with an RSD <3.82%. Stability studies showed that hyperoside was stable in preparation and analytical process. The results indicated that the validated method was successfully used to determine the concentration-time profiles of hyperoside.
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金丝桃苷。该分析方法包括从比格犬血浆中提取金丝桃苷和人参皂苷Re（内标）。色谱分离在Agilent Zorbax XDB-C18（100×2.1 mm，1.8 µm）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2.0分钟。监测的MS/MS离子跃迁，金丝桃苷为4为464.4→463.4，内标为947.12→969.60。金丝桃苷在10至5000 ng/mL范围内获得线性响应。日内和日间精密度（RSD）分别<5.38%和3.39%，提取回收率在94.39%至100.78%之间，RSD<3.82%。稳定性研究表明，金丝桃苷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金丝桃苷的浓度-时间曲线。
