LC-MS/MS法测定大鼠血浆中京尼平苷的浓度  

Determination of Geniposide in Rat Plasma by LC-MS/MS

作　　者：佘丹[1] 苏晓纯[1] 何倩梅[1] 邱昆成 刘奕明[1] 

机构地区：[1]广州中医药大学附属广东省中医院,广东广州510120

出　　处：《中药新药与临床药理》2015年第2期202-205,共4页Traditional Chinese Drug Research and Clinical Pharmacology

基　　金：广东省科技厅资助项目(2011B010500016)

摘　　要：目的建立大鼠血浆中京尼平苷液相色谱-串联质谱（LC-MS/MS）的快速检测方法。方法以芍药苷为内标,血浆样品用甲醇沉淀蛋白法处理,色谱柱为AgilentZORBAXEclipseplus-C18柱（2.1mm×150mm,3.5μm）;流动相为甲醇-5mmol·L^-1乙酸铵（含5mmol·L^-1乙酸）（60∶40）;采用电喷雾离子化（ESI）和正离子多反应离子监测（MRM）方式检测京尼平苷。结果京尼平苷在64.5-12900ng·mL-1浓度范围内线性关系良好,定量下限为64.5ng·mL-1,日内精密度（相对标准偏差,RSD）〈5.2%,日间精密度（RSD）〈11.5%,准确度在98.8%-106.2%之间。结论本研究所建立的LC-MS/MS方法快速、准确、稳定,适用于京尼平苷在大鼠体内的血药浓度测定及药动学研究。Objective To establish a rapid,accurate,and reliable LC-MS/MS method for the determination of geniposide in rat plasma.Methods Paeoniflorin was used as the internal standard.Plasma samples were pretreated by protein precipitation with methanol.Chromatographic separation was carried out on an Agilent ZORBAX Eclipse plus-C18（2.1 mm×150 mm,3.5 μm）column by isocratic elution with methanol- 5 mmol·L^-1ammonium acetate（containing 5 mmol·L^-1acetic acid）（60 ∶40） at a flow rate of 0.2 m L·min-1.Geniposide was detected by the positive electrospray ionization-MS method in multiple reaction monitoring mode.Results A good linear relationship of geniposide was obtained in the concentration range of 64.5 to 12900 ng·m L-1,and the lower limit of quantitation was 64.5 ng·m L-1.The intra-day precision of this method was less than 5.2 %,and the inter-day precision was less than 11.5 %.The relative recoveries ranged from 98.8 % to 106.2 %.Conclusion This assay method is rapid,accurate,and specific,which is suitable for the measurement of plasma geniposide concentration in rats.

关 键 词：京尼平苷 液相色谱-串联质谱法 血药浓度 大鼠 

分 类 号：R285.5[医药卫生—中药学]