目的 建立超高效液相色谱串联三重四级杆飞行时间质谱法(UHPLC-Triple-TOF-MS)快速鉴定松萝中酚酸类有效成分。方法 采用Phenomenex Luna 3u C₁₈色谱柱(150 mm×2.0 mm,3 μm),流动相为甲醇(0.05%甲酸)-水(0.05%甲酸-4 mmol乙酸铵),梯度洗脱,体积流量0.3 mL/min,柱温30 ℃。采用电喷雾离子源负离子模式,全扫描模式采集样品数据,根据高分辨数据并结合二级质谱信息快速鉴定松萝中酚酸类有效成分, 诸如地弗地衣酸、松萝酸、苔色酸等。结果 鉴定出松萝中17种酚酸类有效成分,主要包括缩酚酸类、二苯骈呋喃类、多取代单苯环类化合物,并对其初步裂解规律进行总结。结论 通过UHPLC-Triple-TOF-MS联用技术,为鉴定松萝的化学成分提供了一种快速、高效的定性分析方法。

Objective To establish a quick method of ultra-performance liquid chromatography-quadrupole time-of-fight mass spectrometry (UHPLC-Triple-TOF-MS) for the identification of phenolic acids (diffractaic acid, usnic acid, orsellinic acid, etc.) in Usneae Filum. Methods The separation was performed on the chromatographic column of Phenomenex Luna 3u C₁₈ (150 mm × 2.0 mm, 3 μm), and the mobile phase was methanol (0.05% formic acid)-0.05% formic acid solution (4 mmol ammonium acetate), with a gradient elution at a flow rate of 0.3 mL/min. The column temperature was 30 ℃, and negative ion mode was used for TOF-MS. Results Seventeen compounds were identified or tentatively characterized based on the retention time and MS spectra. They are depsides, two benzo furan, ant multi substituted single benzene as well. And the preliminary fragmentation rules are summarized. Conclusion The results demonstrate that UHPLC-Triple-TOF-MS method is novel, quick, and efficient for the identification of the compounds in Usneae Filum.

国家自然科学基金资助项目(81402894);河北省食品药品监督管理局课题(ZD2015021)