| 引用本文: | 闫佳靓,王海超,张玲,曹桂云,傅春升,田振华.基于UPLC-Q-Exactive Orbitrap MS的秦皮成分分析[J].中国现代应用药学,2023,40(8):1009-1020. |
| YAN Jiajing,WANG Haichao,ZHANG Ling,CAO Guiyun,FU Chunsheng,TIAN Zhenhua.Component Analysis of Fraxini Cortex Based on UPLC-Q-Exactive Orbitrap MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2023,40(8):1009-1020. |
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| 基于UPLC-Q-Exactive Orbitrap MS的秦皮成分分析 |
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闫佳靓1, 王海超1, 张玲1, 曹桂云2, 傅春升3, 田振华4
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1.山东中医药大学药学院, 济南 250300;2.山东宏济堂制药集团股份有限公司, 济南 250100;3.山东中医药大学附属医院, 济南 250014;4.山东中医药大学实验中心, 济南 250300
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| 摘要: |
| 目的 利用超高效液相色谱-四极杆静电场轨道阱高分辨质谱(UPLC-Q-Exactive Orbitrap MS)对秦皮进行成分分析。方法 采用Halo 90Å C18色谱柱(2.1 mm×100 mm，2.7 μm)，以0.05%甲酸水溶液(A)-0.05 %甲酸乙腈溶液(B)为流动相进行梯度洗脱，流速0.3 mL·min-1，柱温30 ℃，进样量5 μL。在电喷雾离子源(ESI)正、负离子模式下采集数据，扫描范围m/z 80~1 200，通过与对照品的保留时间及质谱数据信息对比，并结合精确相对分子质量、质谱裂解规律、质谱数据库(PubChem，ChemicalBook等)及相关文献，对秦皮的化学成分进行快速鉴定。结果 共鉴定出72种化学成分，正离子下19种，负离子下53种，包括香豆素类20种，环烯醚萜类8种，苯乙醇苷类10种，黄酮类17种，有机酸类16种，其他类1种，其中36种成分为首次从秦皮中鉴定出来。结论 本研究建立了秦皮UPLC-Q-Exactive Orbitrap MS的分离鉴定方法，全面阐明了秦皮的化学成分，为秦皮的质量控制与药效物质基础提供了参考。 |
| 关键词: 秦皮 超高效液相色谱-四极杆静电场轨道阱高分辨质谱 成分分析 裂解规律 |
| DOI：10.13748/j.cnki.issn1007-7693.20222148 |
| 分类号:R284.1 |
| 基金项目:国家自然科学基金项目(81774173)；山东省青创人才引育计划 |
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| Component Analysis of Fraxini Cortex Based on UPLC-Q-Exactive Orbitrap MS |
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YAN Jiajing1, WANG Haichao1, ZHANG Ling1, CAO Guiyun2, FU Chunsheng3, TIAN Zhenhua4
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1.School of Pharmacy, Shandong University of Traditional Chinese Medicine, Jinan 250300, China;2.Shandong Hongjitang Pharmaceutical Group Co., Ltd, Jinan 250100, China;3.Affiliated Hospital of Shandong University of Traditional Chinese Medicine, Jinan 250014, China;4.Experimental Center of Shandong University of Traditional Chinese Medicine, Jinan 250300, China
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| Abstract: |
| OBJECTIVE To analyze the composition of Fraxini Cortex by using ultra performance liquid chromatography- quadrupole electrostatic field orbitrap high-resolution mass spectrometry(UPLC-Q-Exactive Orbitrap MS). METHODS Halo 90Å C18(2.1 mm×100 mm, 2.7 μm) as a chromatographic column, 0.05% formic acid aqueous solution(A)-0.05% formic acid acetonitrile(B) was used as the mobile phase for gradient elution. The flow rate was 0.3 mL·min-1, the column temperature was 30 ℃, and the sample volume was 5 μL. The electrospray ionization(ESI) was used to collect data in positive and negative ion modes with the scan range m/z of 80-1 200. Compared with the retention time of reference substance, mass spectrometry data, and combing the accurate relative molecular mass, mass spectrometry fragmentation rule, mass spectrometry databases(PubChem, ChemicalBook, etc.) and related literatures, the chemical components of Fraxini Cortex was identified quickly and accurately. RESULTS A total of 72 chemical constituents were identified in this study, including 20 coumarins, 8 iridoids, 10 phenylethanol glycosides, 17 flavonoids, 16 organic acids and 1 other species, in which 19 compounds in positive ion mode and 53 in negative. Thirty-six of them were identified from Fraxini Cortex for the first time. CONCLUSION This study establishes a UPLC-Q-Exactive Orbitrap MS method for the isolation and identification of compounds in Fraxini Cortex, which can comprehensively elucidate the chemical composition. This study will provide a reference for quality control and the material basis of pharmacological effects of Fraxini Cortex. |
| Key words: Fraxini Cortex UPLC-Q-Exactive Orbitrap MS composition analysis fragmentation pattern |
