采用UPLC-Q-TOF-MS技术鉴定连翘中45种化学成分
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篇名: 采用UPLC-Q-TOF-MS技术鉴定连翘中45种化学成分
TITLE:
摘要: 目的:对连翘药材的化学成分进行结构鉴定。方法:利用超高效液相色谱联用四极杆串联飞行时间质谱(UPLC-Q-TOF-MS)技术对连翘的化学成分进行分析。采用ACQUITY UPLC BEH C18色谱柱,流动相为0.1%甲酸水溶液(A)-0.1%甲酸乙腈溶液(B),梯度洗脱,流速为0.3 mL/min,柱温为30 ℃,进样量为5 μL;采用电喷雾正、负离子模式检测,离子源温度为550 ℃,雾化气体为N2,雾化气、辅助气压力均为379.2 kPa,气帘气压力为241.3 kPa,去簇电压为80 V/-80 V,碰撞能量为35 eV/-35 eV,质量扫描范围为80~1 500 Da。利用Peakview 2.0软件通过所测得成分的一级质谱进行目标性筛查,并计算各成分的高分辨精确分子量,对比对照品图谱以及相关文献,或计算二级质谱中碎片离子的元素组成及分析其裂解途径,推断化合物结构。结果与结论:共鉴定出连翘中的45个化合物,包括7个苯乙醇苷类成分、5个木脂素类成分、5个萜类成分、12个黄酮类成分、7个有机酸类成分、2个酚类成分、2个醌类成分、2个苷类成分和3个其他成分;其中有19个化合物为首次在连翘中得以鉴定。本研究可为连翘药效物质基础的深入研究及其成分的快速定性、定量分析提供基础。
ABSTRACT: OBJECTIVE: To identify chemical components of Forsythia suspense. METHODS: UPLC-Q-TOF-MS technology was used for the chemical components analysis of F. suspense. The determination was performed on ACQUITY UPLC BEH C18 column with mobile phase consisted of 0.1% formic acid aqueous solution (A)- 0.1% formic acid acetonitrile solution (B) with  gradient elution, at the flow rate of 0.3 mL/min; the column temperature was set at 30 ℃; the sample size was 5 μL. Positive and negative ions were detected by electrospray ionization. The temperature of the ion source was 550 ℃; the atomizing gas was N2; the atomizing gas and the auxiliary pressure were 379.2 kPa; the air curtain pressure was 241.3 kPa; the decluster voltage was 80 V/-80 V; the collision energy was 35 eV/-35 eV; the mass scanning range was 80-1 500 Da. Peakview 2.0 software was used to screen the target components by the first-order mass spectrometry, and calculate the high-resolution and accurate molecular weight of each component, compare with the reference spectrum and related literature, or calculate the elemental composition of fragment ions in the second-order mass spectrometry, analyze their decomposition pathways, then infer the structure of compounds. RESULTS & CONCLUSIONS: 45 kinds of compounds were identified from F. suspense,which included 7 phenylethanol glycosides,5 lignans,5 terpenes, 12 flavonoids,7 organic acids,2 phenols,2 quinones,2 glycosides and 3 other components. There were 19 compounds identified for the first time in F. suspense. The study provides a reference for the in-depth study of the pharmacodynamic substance basis of F. suspense and the rapid qualitative and quantitative analysis of the components.
期刊: 2019年第30卷第22期
作者: 周明月,霍金海,孙国东,王伟明
AUTHORS: ZHOU Mingyue,HUO Jinhai,SUN Guodong,WANG Weiming
关键字: 连翘;化学成分;鉴定;超高效液相色谱;四极杆串联飞行时间质谱;苯乙醇苷类;木脂素类
KEYWORDS: Forsythia suspense; Chemical components; Identification; UPLC; Q-TOF-MS; Phenylethanol glycosides; Lignins
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