UPLC-Q-TOF/MS结合指纹图谱在抱龙丸质量控制中的应用

Application of UPLC-Q-TOF/MS Combined with Fingerprint in Quality Control of Baolong Pills

目的:基于UPLC-Q-TOF/MS鉴定抱龙丸中的化学成分,建立UPLC指纹图谱。方法:采用Agilent ZORBAX SB-C_(18)(100 mm×2.1 mm,1.8μm)色谱柱;流动相为0.1%甲酸溶液-乙腈,梯度洗脱;流速为0.2 mL/min;柱温为30℃;进样量为4μL;以ESI为离子源,正、负离子模式分别采集一级、二级质谱数据。采用“中药色谱指纹图谱相似度评价系统(2004 A版)”建立指纹图谱共有模式,并进行相似度评价、聚类分析及偏最小二乘判别分析。结果:通过软件预测及文献数据,从抱龙丸中鉴定出46个成分。指纹图谱确定60个共有峰,13批样品与对照图谱的相似度为0.957~0.995。聚类分析及偏最小二乘判别分析均可将样品分为2类。结论:利用UPLC-Q-TOF/MS法系统阐明抱龙丸中化学成分,结合指纹图谱可为抱龙丸的质量控制提供参考。

Objective:To identify the chemical constituents in Baolong pills based on UPLC-Q-TOF/MS and establish UPLC fingerprint.Methods:Agilent ZORBAX SB-C_(18)column(100 mm×2.1 mm,1.8μm)was used.The mobile phase was 0.1%formic acid solution-acetonitrile with gradient elution,flow rate was 0.2 mL/min,column temperature was 30℃,injection volume was 4μL;Using ESI as the ion source,the first and second order mass spectrum data were collected in positive and negative ion modes,respectively.The common pattern of fingerprint was established by"Similarity evaluation system for chromatographic fingerprint of traditional Chinese medicine(2004 A edition)",similarity evaluation,cluster analysis and partial least squares discriminant analysis were carried out.Results:Forty-six components were identified from Baolong pills by software prediction and literature data.Sixty common peaks were identified in the fingerprint,and the similarity between the 13 batches of samples and reference spectrum was 0.957 to 0.995.Cluster analysis and partial least squares discriminant analysis could divide the samples into two categories.Conclusion:UPLC-Q-TOF/MS method is used to clarify the chemical compositions of Baolong pills,and the combination of fingerprint can provide reference for the quality control of Baolong pills.