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。 OBJECTIVE To establish a HPLC-MS / MS method for the determination of flavone-CN (Fla-CN) in plasma. Methods Tailiroside was used as an internal standard. After the plasma samples were separated by acetonitrile precipitation, the samples were separated on an Agilent XDB-C18 column using acetonitrile-water (65:35) as the mobile phase. The electrospray triple quadrupoles Mass spectrometry was performed in multiple reaction monitoring mode (MRM). The detected ion pairs were m / z 454.0 → 255.0 (Cephalosporin flavone derivative) and 593.2 → 285.1 (tiliroside, internal standard) respectively. Results A good linear relationship was found between 0.5 and 1 000 ng · mL-1 of C. officinale flavonoids in plasma. The intra-and inter-day precision (RSD) was less than 4.6% and the accuracy was within ± 4.1% . In the preclinical pharmacokinetic study, this method was used to test the plasma concentration of oral administration of Cephalosporin flavonoids in SD rats. Conclusion The method for the determination of the concentration of Chlorella vulgaris flavonoids in plasma using high performance liquid chromatography-mass spectrometry has high sensitivity and specificity and is suitable for the study of pharmacokinetics in rats.