[关键词]
[摘要]
目的 采用高效液相色谱-四级杆/静电场轨道阱高分辨质谱(HPLC-Q-Exactive-Orbitrap-MS)法鉴定森登-4味涂剂中化学成分。方法 色谱条件:Shim-pack GIST-HP C18色谱柱(150 mm×4.6 mm,5 μm),流动相为乙腈-0.1%甲酸水溶液,梯度洗脱,体积流量0.35 mL/min,柱温为40 ℃,进样量为5 μL。质谱条件:检测方式Full MS/dd-MS2,扫描范围m/z 110~1 200。电喷雾离子源(ESI),正、负离子模式扫描,喷雾电压4.20 kV(+)、3.80 kV(-),碰撞能量(CE)30 eV。通过全方化学成分信息库,结合多级质谱碎片信息、对照品保留时间,鉴定森登-4味涂剂中化学成分。结果 在森登-4味涂剂中共鉴定出60个成分,包括16个黄酮类成分、13个有机酸类成分、11个环烯醚萜类成分、10个鞣质类成分、4个氨基酸类成分、4个脂肪酸类成分、2个三萜类成分,并考察了山栀苷、槲皮素、阿魏酸、克里拉京、齐墩果酸、脯氨酸、亚油酸的MS2图和可能的裂解途径。结论 对森登-4味涂剂中化学成分进行了快速、准确的鉴定,为其质量标准建立、药效物质挖掘和作用机制研究提供了实验基础。
[Key word]
[Abstract]
Objective To identify the chemical components in Sendeng-4 Pigmentum by HPLC-Q-Exactive-Orbitrap-MS. Methods Chromatographic conditions: Shim-pack GIST-HP C18 column (150 mm × 4.6 mm, 5 μm) was employed with the mobile phase of acetonitrile - 0.1% formic acid solution for gradient elution. The flow rate was 0.35 mL/min, the column temperature was set at 40 ℃, and the volume of sample injection was 5 μL. Mass spectrometry conditions: Detection method: Full MS/dd MS2, scanning range m/z 110 — 1 200. Electrospray ionization (ESI) was applied for scanning positive and negative ion mode scanning with spray voltage 4.20 kV (+) and 3.80 kV (-), and collision energy was 30 eV. Comprehensive chemical composition information database, combined with multi-level mass spectrometry fragment information and reference substance retention time were used to identify the chemical components in Sendeng-4 Pigmentum. Results A total of 60 components were identified in Sendeng-4 Pigmentum, including 16 flavonoids, 13 organic acids, 11 iridoids, 10 tannins, 4 amino acids, 4 fatty acids, and 2 triterpenes. MS2 and possible fragmentation pathway of shanzhiside, quercetin, ferulic acid, corilagin, oleanolic acid, proline, and linoleic acid were investigated. Conclusion Chemical components in Sendeng-4 Pigmentum were quickly and accurately identified, providing an experimental basis for the establishment of its quality standards, the exploration of pharmacological substances, and its mechanism of action.
[中图分类号]
R286.02
[基金项目]
内蒙古自治区自然科学基金资助项目(2022LHQN08001);内蒙古医科大学联合项目(YKD2022LH031);内蒙古医科大学实验室开放基金项目(2022ZN15,2022ZN16);内蒙古医科大学大学生创新创业训练计划项目(202210132052)