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严晟,李漓,黄晨存,赵元,许光明.基于HPLC-Q-Orbitrap-MSn的血三七化学成分分析[J].湖南中医药大学学报英文版,2023,43(6):1042-1048.[Click to copy
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| 基于HPLC-Q-Orbitrap-MSn的血三七化学成分分析 |
| 严晟,李漓,黄晨存,赵元,许光明 |
| (湖南中医药大学, 湖南 长沙 410208) |
| 摘要: |
| 目的 鉴定血三七药材的化学成分。方法 采用HPLC-Q-Orbitrap-MSn技术分析及鉴定血三七中的化学成分。色谱条件：色谱柱为C18柱（250 mm×4.6 mm×5 μm），流动相为0.1%甲酸水-甲醇，梯度洗脱，柱温30 ℃，流速1 mL/min，波长280 nm，进样体积5 μL。质谱条件：加热电喷雾电离源（HESI)；正、负离子检测模式；鞘气60 mL/min；辅助气体流量20 mL/min；喷雾电压3.5 kV；毛细管温度380 ℃；辅助气加热器温度380 ℃；扫描模式：FuLL MS/dd-MS2，FuLL MS分辨率70 000，dd-MS2分辨率17 500；扫描范围m/z 100~1200；碰撞能量为30 eV。数据库、对照品及相关文献比对质谱信息，分析化学元素组成和裂解途径，推断化学结构。结果 鉴定了33种化合物，包括9种酚酸类、6种黄酮类、10种香豆素类、7种苷类和其他类成分1种。结论 从血三七中首次发现了24个化合物，其中1个成分为潜在的新岩白菜素类化合物。 |
| 关键词: 血三七|高效液相色谱|四级杆轨道阱高分辨质谱|鉴定|化学成分 |
| DOI：10.3969/j.issn.1674－070X.２０23.06.012 |
| Received:October 27, 2022 |
| 基金项目:湖南省自然科学基金项目（2021JJ30511）；湖南省中医药科研计划项目（2021062）；湖南省研究生科研创新项目CX20190527）。 |
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| Chemical composition analysis of Xuesanqi based on HPLC-Q-Orbitrap-MSn |
| YAN Sheng,LI Li,HUANG Chencun,ZHAO Yuan,XU Guangming |
| (Hunan University of Chinese Medicine, Changsha, Hunan 410208, China) |
| Abstract: |
| Objective To identify the chemical composition of Xuesanqi （Polygonum amplexicaule D. Don var. sinense Forb）. Methods High-resolution mass spectrometry (HPLC-Q-Orbitrap-MSn) technology was used to identify the chemical composition in Xuesanqi （Polygonum amplexicaule D. Don var. sinense Forb）. Chromatographic conditions were as follows: the column was C18 column [Shimadzu, DiamondiL (250 mm×4.6 mm×5 μm)]; the mobile phase was 0.1% formic acid water-methanol for gradient elution; the column temperature was 30 ℃; the flow rate was 1 mL/min; the wavelength was 280 nm, and the sample volume was 5 μL. Mass spectrometry conditions were established: heated electrospray ionization source (HESI); positive and negative ion detection mode; sheath gas (60 mL/min); auxiliary gas flow (20 mL/min); spray voltage (3.5 kV); capillary temperature (380 ℃); auxiliary gas heater temperature (380 ℃). Samples were analyzed in two scan modes: Full MS (resolution: 70000) and dd-MS2 (resolution: 17500), with can range of m/z100~1200 and collision energy of 30eV. Database, control articles and related literature were used to compare MS spectrometry information, and the chemical element composition and cleavage pathways were analyzed to infer the chemical structure. Results A total of 33 compounds were identified, including 9 phenolic acids, 6 flavonoids, 10 coumarins, 7 glycosides, and 1 other component. Conclusion A total of 24 compounds were first identified from Xuesanqi （Polygonum amplexicaule D. Don var. sinense Forb）, one of these components is a potential new rock cabbage compound. |
| Key words: Xuesanqi （Polygonum amplexicaule D. Don var. sinense Forb）|high performance liquid chromatography|quadrupole orbitrap high-resolution mass spectrometry|identification|chemical composition |
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