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目的:建立测定人血浆中灯盏乙素浓度的HPLC-MS/MS法。方法:采用Platisil ODS色谱柱(250 mm×4.6 mm,5μm),流动相为0.3%甲酸水溶液-甲醇(40∶60),流速为1.0 mL.min-1,以黄芩苷为内标,经乙酸乙酯萃取后,采用电喷雾电离化(ESI)方式和多反应离子监测(MRM)模式进行负离子检测,用于定量分析离子反应分别为m/z 461.1→285.1(灯盏乙素)和m/z 445.1→269.1(黄芩苷)。结果:线性检测范围为0.20～50.00μg.L-1,最低定量浓度0.20μg.L-1,r=0.999 3。低、中、高3个浓度的提取回收率分别为63.5%,69.5%,66.8%,基质效应分别为105.7%,97.5%,96.5%。结论:本法样品处理简单、快速,专属性强,灵敏度高,可用于灯盏乙素在人体内的药代动力学研究。
Objective: To establish a HPLC-MS / MS method for the determination of scutellarin in human plasma. METHODS: Platisil ODS column (250 mm × 4.6 mm, 5 μm) was used. The mobile phase consisted of 0.3% formic acid in methanol (40:60) and the flow rate was 1.0 mL.min-1. Ethyl ester extraction, negative ion detection was performed by electrospray ionization (ESI) and multi-reaction ion monitoring (MRM) mode for the quantitative analysis of ionic reactions m / z 461.1 → 285.1 (scutellarin) and m / z 445.1 → 269.1 (baicalin). Results: The linear range was 0.20 ~ 50.00μg.L-1, the lowest concentration was 0.20μg.L-1, r = 0.999 3. The recoveries of low, medium and high concentrations were 63.5%, 69.5% and 66.8%, respectively. The matrix effects were 105.7%, 97.5% and 96.5% respectively. Conclusion: The sample is simple, rapid, specific and sensitive. It can be used to study the pharmacokinetics of scutellarin in human.