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目的:建立一种可靠的灯盏乙素定量分析方法。方法:用三级四极串联质谱(MS/MS)作为HPLC的检测器,其中MS/MS使用了多反应监测(MRM)扫描方式。选择母→子离子对m/z-461→m/z-285作为MRM监测的离子对;HPLC流动相为100%甲醇,流速09mL·min-1,色谱柱BeckmanODS1。以测定短葶飞蓬提取物的灯盏乙素含量为例,对此方法进行了应用。结果:灯盏乙素在短葶飞蓬提取物中含量为698%。方法线性范围20~160ng·mL-1(γ=0999);加入灯盏乙素标准品20,60和160ng的加样回收率分别为:965%,974%和973%。检测限为1ng,每个样品的分析时间为4min。结论:此法灵敏、快速、准确,可应用于灯盏乙素的各种药剂、药代的研究。
Objective: To establish a reliable method for quantitative analysis of scutellarin. Methods: Three-stage quadrupole tandem mass spectrometry (MS/MS) was used as a detector for HPLC, where MS/MS used multiple reaction monitoring (MRM) scans. The mother-ion pair m/z-461→m/z-285 was selected as the MRM monitored ion pair; the HPLC mobile phase was 100% methanol with a flow rate of 09 mL·min-1 and the column Beckman ODS1. This method was applied to the determination of scutellarin content of E. sinensis extract as an example. RESULTS: The content of scutellarin in the extract of Erigeron breviscapus was 698%. The linear range of the method was 20-160 ng·mL-1 (γ=0999). The recoveries of 20, 60, and 160 ng of scutellarin added were: 965%, 974%, and 973%, respectively. The detection limit was 1 ng and the analysis time for each sample was 4 min. Conclusion: This method is sensitive, rapid and accurate and can be applied to the study of various agents and pharmacokinetics of scutellarin.