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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 |
| 阅读数： | 401 次 |
| 本月下载数： | 19 次 |
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