银杏叶片UPLC指纹图谱检测方法的建立及其在质量控制中的应用

目的:建立银杏叶片的超高效液相色谱(UPLC)指纹图谱检测方法,快速评价银杏叶片质量。方法:采用UPLC® H-Class超高效液相色谱系统,Acquity UPLC® HSST3色谱柱(2.1 mm×100 mm,1.8 μm),以乙腈-0.4%磷酸溶液为流动相,梯度洗脱,流速0.4 mL·min^-1,检测波长360 nm,柱温40 ℃,进样量1 μL。结果:本方法采用UPLC,18 min内完成银杏叶片的指纹图谱分析,主要成分芦丁、槲皮素、山柰素、异鼠李素等色谱峰分离良好,方法精密度、重复性、稳定性的相似度均>0.996,耐用性试验的RSD小于2%;结合相似度评价方法(SE)和聚类分析(HCA)、主成分分析(PCA),将12个厂家的68批次样品分为2类,可以区分出异常样本。结论:建立的UPLC指纹图谱检测方法高效、快速、准确,专属性强,为其质量控制及评价提供了更加有效的可行方法。

Objective:To establish the UPLC fingerprint of Yinxingye tablets for quality evaluation of Yinxingye tablets rapidly.Methods:The samples were analyzed by UPLC with Acquity UPLC® HSST3 column(2.1 mm×100 mm, 1.8 μm).The mobile phase consisted of acetonitrile and 0.4% phosphoric acid aqueous solution with gradient elution mode at the flow rate of 0.4 mL·min^-1.The column temperature was 40 ℃,the detection wavelength was set at 360 nm,and the injection volume was 1 μL.Results:The UPLC was used to develop fingerprint of Yinxingye tablets within 18 min.The main peaks were separated clearly for rutin,quercetin,kaempferide,isorhamnetin,et al.The similarity of precision,reproducibility and stability were more than 0.996.Robustness was below 2%.Based on these methods including similarity evaluation(SE),hierarchical cluster analysis(HCA)and principal component analysis(PCA),68 batches of Yinxingye tablets from 12 companies were divided into 2 clusters by their quality difference.Conclusion:A high-performance,rapid,accurate and exclusive method of UPLC fingerprint was developed,which can be used for quality control and evaluation.