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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 To separate and analyze the constituents of the methanol extract of Chinese coltsfoot flower by UPLC-Q-TOF-MS in both anions and anions using ultra performance liquid chromatography (UPLC-MS). Methods Agilent Poroshell 120 EC-C 18 column (100 mm × 2.1 mm, 2.7 μm) with 0.1% formic acid in water (A) and acetonitrile (B) as the mobile phase. Positive ion mode: gradient elution 0 to 1 min, 5 to 17% B; 1 to 3 min, 17 to 19% B; 3 to 14 min, 19 to 44% B; ~ 66% B; 16 ~ 26 min, 66% ~ 87% B; 26 ~ 28 min, 87% ~ 95% B; Negative ion mode: gradient elution 0 to 2 min, 5% to 14% B; 2 to 10 min, 14% to 32% B; 10 to 15 min, 32% Volume flow 0.4 mL / min, injection volume 5 μL. Compound information is analyzed by positive and negative ion mass spectrometry information, elemental composition, and the relative retention time and mass spectral data of the compounds in the reference or literature. Results According to the accurate relative molecular mass of the compound provided by UPLC-Q-TOF-MS, 34 compounds were identified, including 12 terpenoids, 8 flavonoids, 7 phenolic acids, benzopyran compounds 2, 1 benzofuran, 1 aliphatic ketone and 3 alkaloids. Conclusion This method provides a theoretical basis for the quality control of Colletotrichum and its rational clinical application, and provides a reference for elucidating the substance basis of its efficacy.