HPLC-Q-Exactive-Orbitrap-MS法鉴定森登-4味涂剂中化学成分

Identification of chemical components in Sendeng-4 Pigmentum by HPLC-QExactive-Orbitrap-MS

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 C_(18)色谱柱(150 mm×4.6 mm,5μm),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5μL。质谱条件:检测方式Full MS/dd-MS^(2),扫描范围m/z110~1 200。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。

Objective To identify the chemical components in Sendeng-4 Pigmentum by HPLC-Q-Exactive-Orbitrap-MS.Methods Chromatographic conditions:Shim-pack GIST-HP C_(18) column(150 mm×4.6 mm,5μm)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 5μL.Mass spectrometry conditions:Detection method:Full MS/dd MS^(2),scanning range m/z 110—1200.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. ConclusionChemical 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.