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UPLC-Q-TOF-MS法鉴定消肿止痛液有效部位的化学成分
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| 篇名： | UPLC-Q-TOF-MS法鉴定消肿止痛液有效部位的化学成分 |
| TITLE： | |
| 摘要： | 目的：分析消肿止痛液有效部位的化学成分，为阐明其药效物质基础及将其二次开发为软膏制剂提供依据。方法：采用超高效液相色谱-四级杆-飞行时间质谱联用（UPLC-Q-TOF-MS）法对消肿止痛液有效部位（经D101大孔树脂分离得到的40％乙醇洗脱部位）进行成分分析。色谱条件为采用Hypersil GOLD aQ C18色谱柱，以0.1％甲酸乙腈（A）-0.1％甲酸水（B）为流动相进行梯度洗脱，流速0.4 mL/min，进样量4 μL，柱温30 ℃；质谱条件为采用电喷雾离子源（ESI）在正/负离子扫描模式（ESI+/ESI－）下进行检测，扫描范围100～2 000 Da，碰撞能量45/－45 eV，扩展碰撞器能量10/15 eV。获得图谱后收集化合物的精确分子量、保留时间和多级碎片离子信息，通过与对照品质谱信息及参考文献比对进行化学成分鉴定。结果：共鉴定出48个化合物，在ESI+、ESI－检测模式下分别鉴定出9、39个。其中，酚酸类成分10个、苯丙素类成分8个、蒽醌类成分9个、黄酮类成分3个、生物碱类成分7个、鞣质类成分5个、其他类成分6个。结论：UPLC-Q-TOF-MS法可快速、高效、准确地鉴定消肿止痛液有效部位的化学成分，该部位的主要化学成分为酚酸类、苯丙素类、蒽醌类、生物碱类和鞣质类。 |
| ABSTRACT： | OBJECTIVE： To analyze chemical components in active fraction of Xiaozhong zhitong lotion， to clarify the material basis of its efficacy， and to provide reference for the second development of ointment preparation. METHODS： UPLC-Q-TOF-MS was adopted to analyze the chemical components of active fraction （40％ ethanol elution site separated by D101 macroporous resin） of Xiaozhong zhitong lotion. The determination was performed on Hypersil GOLD aQ C18 column with mobile phase consisted of 0.1％ formic acid acetonitrile （A）-0.1％ formic acid water （B） （gradient elution） at the flow rate of 0.4 mL/min. The sample size was 4 μL， and the column temperature was 30 ℃. The condition of mass spectrometry was ESI detection in positive and negative scanning ion mode （ESI+/ESI－）. The scanning range was 100-2 000 Da. The collision energy was 45/－45 eV， and the energy of the extended collider was 10/15 eV. The accurate molecular weight， retention time and multi-stage fragment ion information of the compounds were collected after obtaining the chromatogram， and the chemical components were identified by comparing with the mass spectrum information of reference materials and references. RESULTS： A total of 48 compounds were identified， and 9 and 39 compounds were identified under ESI+/ESI－ ion mode， mainly including 10 phenolic acids， 8 phenylpropanoids， 9 anthraquinones， 3 flavones， 7 alkaloids， 5 tannins and 6 other categories. CONCLUSIONS： UPLC-Q-TOF- MS method is rapid， efficient and accurate for identify chemical components from active fraction of Xiaozhong zhitong lotion. Main chemical components of the active fraction are phenolic acids， phenylpropanoids， anthraquinones， alkaloids and tannins. |
| 期刊： | 2019年第30卷第23期 |
| 作者： | 王银洁，刘本臣，刘军，莫家欣，胡安琪，刘嘉琪，冯倩仪，宫凯敏 |
| AUTHORS： | WANG Yinjie，LIU Benchen，LIU Jun，MO Jiaxin，HU Anqi，LIU Jiaqi，FENG Qianyi，GONG Kaimin |
| 关键字： | 消肿止痛液；有效部位；超高效液相色谱-四级杆-飞行时间质谱联用法；化学成分；鉴定 |
| KEYWORDS： | Xiaozhong zhitong lotion； Active fraction； UPLC-Q-TOF-MS； Chemical components； Identification |
| 阅读数： | 377 次 |
| 本月下载数： | 4 次 |
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