利用超高效液相色谱-四级杆飞行时间串联质谱法(UPLC-QTOF-MS/MS)对中药卷柏的化学成分进行快速分析及鉴定.采用Agilent Poroshell 120 SB-Aq(2.7 µm,2.1 mm × 100 mm)色谱柱,以乙腈-0.1％甲酸水溶液为流动相,梯度洗脱,流速为0.4mL/min,进样量为3 μL;选择电喷雾离子源分别在正、负离子模式下扫描分析,通过保留时间、精确相对分子质量和二级质谱裂解碎片,对所得成分的主要色谱峰进行鉴定.结果显示从卷柏中共鉴定出54个化学成分,主要包括双黄酮及黄酮类15个、炔酚类12个、酚酸类10个、苯丙素类5个、甾体类2个、萜类2个、氨基酸及肽类2个、酯类2个和其他类4个,并首次探讨炔酚类成分的裂解规律.该研究建立的UPLC-QTOF-MS/MS方法可以快速准确且较全面地分析鉴定卷柏中的化学成分,可为其质量控制及药效物质基础研究提供科学依据.
Abstract
Ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-QTOF-MS/MS)was employed to rapidly analyze and identify the chemical constituents of Selaginellae Herba.An Agilent Poroshell 120 SB-Aq(2.7 µm,2.1 mm × 100 mm)chromatographic column was used with acetonitrile-0.1％formic acid aqueous so-lution as the mobile phase in gradient elution,at a flow rate of 0.4 mL/min and an injection volume of 3 μL.The electrospray ion source was selected to scan analyze in both positive and negative ion modes.The main chromatographic peaks of the ob-tained constituents were identified through retention time,accurate relative molecular mass,and secondary mass spectrometry fragmentation.A total of 54 compounds were identified in Selaginellae Herba,including 15 biflavonoids and flavonoids,12 se-laginellins,ten phenolic acids,five benzenepropanoids,two steroids,two terpenoids,two amino acids and peptides,two esters,and four other categories.The UPLC-QTOF-MS/MS method established in this study can rapidly,accurately,and comprehen-sively analyze and identify the chemical constituents in Selaginellae Herba,providing a scientific basis for its quality control and pharmacological substance basis research.
维普
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