基于UHPLC-Q-Exactive Orbitrap MS的芪龙壮儿口服液指纹图谱研究

Study on Fingerprint of Qilong Zhuang'er Oral Liquid(芪龙壮儿口服液)Based on UHPLC-Q-Exactive Orbitrap MS

目的:建立芪龙壮儿口服液UHPLC-Q-Exactive Orbitrap MS正、负离子两种检测模式下的指纹图谱,为该制剂的质量控制提供参考和依据。方法:采用Thermo Accucore aQ RP18(2.1 mm×150 mm,2.6μm)色谱柱进行色谱分离,加热电喷雾离子源正、负离子同时检测。根据一级准分子离子精确质荷比、二级质谱碎片离子信息、文献报道和对照品比对鉴定共有峰成分。结果:构建了芪龙壮儿口服液正、负离子模式下的指纹图谱共有模式并分别确认了24(正离子模式)和17(负离子模式)个共有指纹峰。10批芪龙壮儿口服液指纹图谱与对照指纹图谱的相似度分别大于0.986(正离子模式)和0.968(负离子模式)。在正离子模式下鉴定了15个共有峰,其中9个共有峰采用对照品确认;负离子模式下鉴定了12个共有峰,其中9个共有峰采用对照品确认。结论:所建立的芪龙壮儿口服液正、负离子两种模式下的指纹图谱,结合共有峰的高分辨质谱定性分析,从正、负两个维度较为全面地表征了该制剂的化学成分指纹特征,为芪龙壮儿口服液的质量评价提供了依据和方法。

Objective:To establish the UHPLC-Q-Exactive Orbitrap MS fingerprint of Qilong Zhuang'er Oral liquid in positive and negative modes,so as to provide reference and basis for the quality control of the preparation.Methods:The separation was performed on a Thermo Accucore aQ RP18(2.1 mm×150 mm,2.6μm).The heated the electric spray ion source and positive and negative modes were applied.The common peaks were identified based on accurate MS data,fragmentation characteristics of MS2,published literature and reference standards.Results:The fingerprint of Qilong Zhuang'er oral liquid in both of positive and negative modes were constructed,and 24(positive ion mode)and 17(negative ion mode)common peaks were identified respectively.The similarity between the fingerprint of 10 batches of Qilong Zhuang'er oral liquid and the control fingerprint is greater than 0.986(positive mode)and 0.968(negative mode),respectively.Totally 15 common peaks were identified by high resolution mass spectrometry in positive mode,among which nine common peaks were identified by comparing with reference substances.Among the 12 common peaks identified in negative mode,nine common peaks were identified by comparing with reference substances.Conclusion:The fingerprint of Qilong Zhuang'er oral liquid in positive and negative modes established by UHPLC-Q-Exactive Orbitrap MS technology combined with qualitative analysis of common peaks,comprehensively characterized the chemical composition fingerprint of the preparation from both of the positive and negative dimensions.It can provide basis and method for the quality evaluation of Qilong Zhuang'er oral liquid.