液相色谱-电喷雾质谱定量测定银杏内酯的研究

Quantitative determination of ginkgolides by liquid chromatography-electrospray mass spectrometry

目的:研究了用液相色谱-电喷雾质谱联用技术定量测定4种银杏内酯的方法.方法:采用ZOR-BAXRX-C18(2.1 mm×150 mm)色谱分析柱,梯度洗脱,0 min时,流动相甲醇-水(25:75),25min,甲醇-水(35:65);柱温25℃;流速0.25 mL·min-1,采用电喷雾负模式[ESI(Neg)]、选择离子采集方式[SIM]定量测定了银杏内酯A,B,C和白果内酯BB.结果:该方法测定银杏内酯的线性范围为4.04～1.01×102ng,r为0.993 7～0.999 8,RSD为2.50%～4.73%.选择离子采集方式的检测限可达1.47×10-3～0.320μg·mL-1.结论:该方法稳定、可靠,能快速定量测定微量银杏内酯.

Objective： This paper reports a method based on liquid chromatography coupled with electrospray mass spectrometry for the analysis of terpenoids in ginkgo laminae. Method： The analysis was performed on ZORBAX RX-CIs（2.1 nm× 150 nm）column with methanol-water（with gradient） as mobile phase at a flow rate of 0.25 mL·min^-1,and column temperature of 25 ℃ .Analyses were carried out in the selected ion monitoring （SIM） mode. Result： Ginkgolides （GA, GB and GC） and bilobalide were quantitatively detected by external standardization with linear in the range of 4.04-1.012× 10^2 μg, with coefficient and relative standard deviations being 0.993 7-0.999 8 and 2.50%-4.73%. LC-ESI-MS shows a greatly increased sensitivity compared with other methods. The detection limit of this method by SIM was 1.47x 10^-3-0.320μg·mL^-1. Conclusion： This method is specific, reproducible, rapidly and permits quantitative analyses of ginkgolides and bilobalide in different samples with simple pre-purification steps.