基于超高效液相色谱－四极杆串联飞行时间质谱的克咳片化学成分快速识别研究

Rapid Identification of Constituents in Keke Tablets by High-performance Liquid Chromatography－Quadrupole Time-of-flight Mass Spectrometry

中文关键词:克咳片  超高效液相色谱－四极杆串联飞行时间质谱（UPLC－Q－TOF MS）  物质基础  定性分析

Key Words:Keke Tablets  high-performance liquid chromatography－quadrupole time-of-flight mass spectrometry（UPLC－Q－TOF MS）  material basis  qualitative analysis

中文摘要:采用超高效液相色谱－四极杆串联飞行时间质谱（UPLC－Q－TOF MS）技术对克咳片甲醇－水提取物中的化学成分进行鉴定。克咳片提取物经Waters CORTECS T3 （150 mm × 2.1 mm，1.6 μm）色谱柱分离，以乙腈－0.1%甲酸水进行梯度洗脱，正负离子模式下采集得到其总离子流图。对色谱图中的各色谱峰进行精确质量数识别。通过自建的质谱数据库、化合物质谱裂解规律，并结合相关文献及对照品的保留时间与质谱信息，对克咳片甲醇－水提取物中的主要成分进行定性分析。共鉴定出94个化学成分，其中生物碱类33个、黄酮类22个、苯丙素类9个、三萜皂苷类8个、氨基酸类5个、氰苷类3个、有机酸类6个以及其他类化合物8个。该研究全面分析了克咳片的化学成分，为克咳片药效的物质基础研究与质量控制提供了科学依据。

Abstract:A high-performance liquid chromatography－quadrupole time-of-flight mass spectrometric（UPLC－Q－TOF MS） method was established to identify the constituents in Keke Tablets．The analytes was separated on a waters CORTECS T3 column（150 mm × 2.1 mm，1.6 μm） by gradient elution，with 0.1% formic acid water－acetonitrile as the mobile phase，and then analyzed in both positive and negative ions modes．Constituents in methanol－H2O extract of Keke tablets were identified by mass spectrometry database，fragmentation regularities of mass spectra，consulting literature reports，retention time and mass data of reference compounds．A total of 94 constituents were identified，including 33 alkaloids，22 flavones，9 phenylpropanoids，8 triterpenoid saponins，5 amino acids，3 cyanophoric glycosides，6 organic acids and 8 other compounds．Chemical constitutions of Keke tablets were comprehensively analyzed，which will be helpful to the quality control and pharmacodynamics material basis research.