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林美妤,袁志鹰,曾琪,何瑶,肖碧霞,李怡杰,杜琪,陈乃宏.基于UPLC-Q-TOF-MSE的百合化学成分分析[J].湖南中医药大学学报英文版,2020,40(8):964-973.[Click to copy
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| 基于UPLC-Q-TOF-MSE的百合化学成分分析 |
| 林美妤,袁志鹰,曾琪,何瑶,肖碧霞,李怡杰,杜琪,陈乃宏 |
| (湖南中医药大学药学院, 湖南 长沙 410208;湖南省中药饮片标准化及功能工程技术研究中心, 湖南 长沙 410208;湖南中医药大学药学院, 湖南 长沙 410208;湖南省中药饮片标准化及功能工程技术研究中心, 湖南 长沙 410208;中国医学科学院北京协和医学院药物研究所, 北京 100050) |
| 摘要: |
| 目的 利用超高效液相色谱-四极杆-飞行时间质谱（UPLC-Q-TOF-MSE）技术对百合的化学成分进行定性分析。方法 液相采用Acquity超高效液相色谱，Waters Acquity UPLC BEH C18（2.1 mm×100 mm，1.7 μm）色谱柱，乙腈-0.1%甲酸水溶液为流动相梯度洗脱，流速0.4 mL/min，柱温35℃，进样量10 μL；质谱采用Xevo G2-XS型四级杆飞行时间质谱仪，电喷雾离子源正、负离子模式下采集数据。通过分析一级质谱精确相对分子质量和二级质谱裂解信息，结合对照品与文献报道进行鉴定和推测。结果 从百合中初步鉴定了33个化合物，23个酚酸类化合物，8个甾体皂苷类化合物，2个生物碱类化合物。其中(25R)-呋甾烷-5-烯-1β,3α,22α,26-四醇-3,26-O-β-D-吡喃葡萄糖苷、(25R)-26-O-β-D-吡喃葡萄糖-5α-呋甾烷-3β,20α,26-三醇-3-O-α-L-吡喃鼠李糖(1→2)-β-D-吡喃葡萄糖苷、(25R)-螺甾烷-5-烯-3β,17α-二醇-3-O-α-L-吡喃鼠李糖(1→2)-β-D-葡萄糖苷均首次在该植物中发现。结论 UPLC-Q-TOF/MSE技术能全面、快速地对百合化学成分进行分析，为其药效物质基础和质量控制的进一步阐明奠定了良好的基础。 |
| 关键词: 百合 化学成分 UPLC-Q-TOF-MSE 酚酸 甾体皂苷 生物碱 |
| DOI：10.3969/j.issn.1674-070X.2020.08.011 |
| Received:February 16, 2020 |
| 基金项目:湖南中医药大学一流学科项目（201803）；湖南省中药饮片标准化及功能工程技术研究中心开放基金项目（0101003004）；湖南中医药大学2019年大学生创新创业训练计划项目（2019-100）。 |
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| Analysis of Chemical Constituent of Lilium broumii by UPLC-Q-TOF-MSE |
| LIN Meiyu,YUAN Zhiying,ZENG Qi,HE Yao,XIAO Bixia,LI Yijie,DU Qi,CHEN Naihong |
| (College of Pharmacy, Hunan University of Chinese Medicine, Changsha, Hunan 410208, China;Hunan Engineering Technology Center of Standardization and Function of Chinese Herbal Decoction Pieces, Changsha, Hunan 410208, China;College of Pharmacy, Hunan University of Chinese Medicine, Changsha, Hunan 410208, China;Hunan Engineering Technology Center of Standardization and Function of Chinese Herbal Decoction Pieces, Changsha, Hunan 410208, China;Institute of Materia Medica, Chinese Academy of Medical Sciences and Peking Union Medical College, Beijing 100050, China) |
| Abstract: |
| Objective To perform qualitative analysis of the chemical constituents of Lilium broumii by UPLC-Q-TOF-MSE. Methods Acquity ultra-high performance liquid chromatography was used. Waters Acquity UPLC BEH C18 (2.1 mm×100 mm, 1.7 μm) was used in the liquid phase. The mobile phase consisting of acetonitrile-0.1% formic acid was used for gradient elution. The volume flow rate was 0.4 mL/min, column temperature was 35℃, and the sample volume was 10 μL. The Xevo G2-XS quadrupole time-of-flight mass spectrometer was used to collect data by positive and negative ionization modes with electro-spray ionization source. By analyzing the accurate relative molecular mass of the first-level mass spectrometer and the information of the second-level mass spectrometry cleavage, identification and speculation were performed combined with the reference substance and literature reports. Results Totally 33 compounds including 23 phenolic acids, 8 steroidal saponins and 2 alkaloids were initially identified from Lilium broumii. Among them, (25R)-furost-5-en-1β, 3α, 22α, 26-tetrol-3, 26-di-O-β-D-Gls, (25R)-26-O-β-D-Glc-5α-furost-3β, 22α, 26-triol-3-O-α-L-Rha-(1→2)-β-D-Gls and (25R)-spirost-5-ene-3β, 17α-diol-3-O-α-L-Rha-(1→2)-β-D-Gls were firstly discovered in Lilium broumii. Conclusion UPLC-Q-TOF/MSE can analyze the chemical components of Lilium broumii comprehensively and quickly. This study lays a good foundation for the further elucidation of the pharmacodynamic material basis and quality control of Lilium broumii. |
| Key words: Lilium broumii chemical constituents UPLC-Q-TOF/MSE |
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