UPLC-Q-TOF-MS法分析款冬花的化学成分

Analysis on chemical composition of Farfarae Flos by UPLC-Q-TOF-MS

目的应用超高效液相色谱仪联用四级杆串联飞行时间质谱仪(UPLC-Q-TOF-MS)在正负离子模式下分离分析款冬花药材甲醇提取物成分。方法 Agilent Poroshell 120 EC-C_(18)色谱柱(100 mm×2.1 mm,2.7μm),以0.1%甲酸水(A)-乙腈(B)溶液为流动相。正离子模式:梯度洗脱0~1 min,5%~17%B;1~3 min,17%~19%B;3~14 min,19%~44%B;14~16 min,44%~66%B;16~26 min,66%~87%B;26~28 min,87%~95%B;28~33 min,95%B。负离子模式:梯度洗脱0~2 min,5%~14%B;2~10 min,14%~32%B;10~15 min,32%B。体积流量0.4 mL/min,进样量5μL。通过正、负离子质谱信息,元素组成以及比对对照品或文献中化合物的保留时间和质谱数据等分析化合物信息。结果结合UPLC-Q-TOF-MS提供的化合物准确相对分子质量共鉴定款冬花提取物中34个化合物,包括萜类12个、黄酮类8个、酚酸类7个、苯并吡喃类化合物2个、苯并呋喃类1个、脂肪酮类1个和生物碱3个。结论该方法为款冬花的质量控制及临床的合理应用提供了理论依据,为阐明其药效物质基础提供参考。

Objective The chemical constituents in the methanol extract from Farfarae Flos were rapidly identified using UPLC-Q-TOF-MS in positive and negative ion modes. Methods The analysis was performed on an Agilent Poroshell 120 EC-C18 chromatographic column （100 mm x 2.1 mm, 2.7 pm）. The mobile phase consisted of acetonitrile and 0.1% aq formic acid. In positive ion mode, gradient elution： 0---1 min, 5%--17% B; 1--3 rain, 17%--19% B; 3--14 min, 19%--44% B; 14--16 min, 44%--66% B; 16--26 min, 66%--87% B; 26--28 min, 87%--95% B; 28--33 min, 95% B. In negative ion mode, gradient elution： 0--2 min, 5%--14% B; 2--10 min, 14%--32% B; 10--15 min, 32% B. The flow rate was 0.4 mL/min, and the injection volume was 5μL. The information of the compounds was analyzed by positive and negative ion modes mass spectrum information, elements composition, reference substance retention time or mass spectrum parameters of compounds in literature. Results Thirty-four compounds in Farfarae Flos extracts were identified, combined with provided accurate molecular weight compounds by UPLC-Q-TOF-MS, including 12 kinds of terpenoids, eight kinds of flavonoids, seven kinds of phenolic acids, two kinds of pyran compounds, one kind of phenolic ketones, one kind of fat ketones, and three kinds of alkaloids. Conclusion The method provides the theory basis for quality control and the clinical reasonable application and provides the reference for clarifying its efficacy material base.