【摘要】 目的建立测定血浆中委陵菜黄酮衍生物(flavone-CN,Fla-CN)的高效液相色谱-质谱联用(LC-MS/MS)分析方法。方法以委陵菜黄酮(tiliroside)为内标,血浆样品经乙腈沉淀蛋白后,以乙腈-水(65∶35)为流动相,用Agilent XDB-C18柱分离,通过电喷雾三重四级杆串联质谱,以多反应监测模式(MRM)进行检测,检测离子对分别为m/z 454.0→255.0(委陵菜黄酮衍生物)和593.2→285.1(tiliroside,内标)。结果血浆中委陵菜黄酮衍生物在0.5~1 000 ng·mL-1内呈现良好的线性关系,方法的日内和日间精密度(RSD)均小于4.6%,准确度在±4.1%之内。在临床前药动学研究中,应用此方法测试了SD大鼠口服给药委陵菜黄酮衍生物后的血药浓度。结论应用高效液相色谱-质谱联用技术建立的测定血浆中委陵菜黄酮衍生物浓度的方法灵敏度高、专属性强,适用于大鼠体内药动学研究。更多还原

【Abstract】 OBJECTIVE To establish an LC-MS /MS method for determination of Fla-CN in plasma. METHODS Tiliroside from Potentilla chinensis Ser. was used as the internal standard. After protein precipitation by acetonitrile,samples were separated on Agilent XDB-C18column by using acetonitrile-water( 65∶ 35) as mobile phase. The quantitation was performed on an LC-MS / MS with negative electrospray ionization in multiple reaction monitoring( MRM) mode. Fla-CN was detected at m / z 454. 0→255. 0,tiliroside( IS) at m/z 593. 2→285. 1. RESULTS Linear calibration curves were obtained in the concentration range of 0. 5-1 000 ng·mL- 1 for Fla-CN. The inter-day and intra-day precision values( RSD) were below 4. 6%,and the accuracy( relative error) was within ± 4. 1%. The method was used to determine the plasma concentration of Fla-CN after oral administration in SD rats in a predinical pharmacokinetic study. CONCLUSION The LC-MS / MS method for determination of Fla-CN in plasma is sensitive,specific and suitable for the pharmacokinetic study of Fla-CN in rats.更多还原