银杏酮酯黄酮类成分指纹图谱分析方法建立

摘要

Objective:To develop an analysis method for establishment of the fingerprint of Ginkgo Biloba Extract 50 (GBE50) and Ginkgo Biloba Tablets based on HPLC-DAD,and obtain the common peaks of 10 batches of GBES0 samples using a UPLC/QTOF-MS analysis method combined with an automated MSE technique.Methods:Agilent Poroshell 120 SB C1s column (4.6 mm × 150 mm,2.7 μm) was used as the separation column.Gradient elution was performed using mobile phase consisting of 0.1％ phosphoric acid and acetonitrile.The flow rate was 1 mL · min-1,detecting wave length was 254 nm and column temperature was 35 ℃.Results:The fingerprint was established.Meanwhile,41 common peaks were identified in the assistance of LC-MS.Conclusion:The fingerprint of GBE50 and Ginkgo Biloba tablets were established to improve the quality standards and provide new methods for quality evaluation.%目的:利用HPLC-DAD建立一个适用于银杏酮酯提取物(总黄酮和内酯含量达到50％的银杏叶提取物,简称GBE50)及银杏酮酯片中黄酮类成分指纹图谱的分析方法,并运用UPLC/ESI-QTOF-MS结合MSE技术进一步指认10批次银杏酮酯提取物指纹图谱中共有峰.方法:采用Agilent Poroshell 120 SB C1s色谱柱(150 mm ×4.6 mm,2.7 μm),检测波长254 nm,参比波长450 nm,参比带宽20 nm;柱温35℃;流速1 mL· min-;进样量10 μL;流动相以0.1％磷酸-水溶液为A相,乙腈溶液为B相进行梯度洗脱.结果:以10个批次的银杏酮酯提取物为样品建立了银杏酮酯提取物的指纹图谱,相似度均＞0.90;并通过液质联用分析方法指认出其中41个共有峰成分.结论:建立的指纹图谱方法可整体评价银杏酮酯提取物药品质量,对银杏酮酯提取物及其制剂银杏酮酯片内在成分进行全面分析,为质量评价提供新手段.