摘要
目的 基于高效液相色谱–四级杆/静电场轨道阱高分辨质谱(HPLC-Q-Exactive-MS)技术对巴特日七味丸中化学成分分析鉴定。方法 使用Agilent Zorbax SB-Aq色谱柱(150 mm×4.6 mm,5μm),流动相为甲醇–0.1%甲酸水溶液,梯度洗脱,体积流量为0.35 mL/min,柱温为35℃,进样量为10μL。采用电喷雾离子源(ESI),检测方式:Full MS/dd-MS2,Full MS分辨率:70 000,dd-MS2分辨率:17 500,扫描范围:m/z 110~1 200。喷雾电压:3.80 kV(+)、3.20 kV(-),碰撞能量:30 eV,离子传输管温度:300℃(+)、400℃(-),辅助气体积流量:30 L/min,辅助气温度:350℃。利用Thermo Xcalibur 3.0软件对在正、负离子模式下获得的总离子流数据进行处理,以各成分保留时间、元素组成、多级质谱碎片信息、与部分对照品比对做进一步确认。结果 共鉴定出81个化学成分,包括29个生物碱类成分、16个黄酮类成分、12个有机酸类成分、9个没食子酸酯类成分、5个倍半萜类成分、3个鞣质类成分、4个脂肪酸类成分、3个氨基酸类成分,其中10个成分经与对照品比对得到进一步确证。并考察了槲皮素、新乌头原碱、莽草酸、没食子酰葡萄糖、克里拉京、去氢木香内酯、L-脯氨酸、亚油酸的MS2图和可能的裂解途径。结论 HPLC-Q-Exactive-MS技术可对巴特日七味丸中成分进行了快速、全面的定性分析,为巴特日七味丸的药效物质研究提供参考。
Objective To analyze and identify the chemical constituents in Bateri Qiwei Pills based on HPLC-Q-Exactive-MS.Methods The separation was performed on Agilent Zorbax SB-Aq column(150 mm×4.6 mm,5μm)with the mobile phase of methanol-0.1%formic acid aqueous solution by gradient elution.The flow rate was 0.35 mL/min,column temperature was 35℃,and the volume of sample injection was 10μL.Electrospray ionization(ESI)was used.The detection mode was Full MS/dd MS2,the resolution of Full MS was 70000,the resolution of dd-MS2 was 17500,and the scanning range was m/z 110—1200.Spray voltage was 3.80 kV(+)and 3.20 kV(-),collision energy was 30 eV,ion transfer tube temperature was 300℃(+)and 400℃(-),auxiliary gas volume flow was 30 L/min,and auxiliary gas temperature was 350℃.Total ion flow data obtained in both positive and negative ion modes were analyzed by Thermo XCalibur 3.0 software,and further confirms were carried on by retention time of each component,elemental composition,multi-level mass spectrometry fragment information,with comparison with some reference materials.Results A total of 81 components were identified in Bateri Qiwei Pills,including 29 alkaloids,16 flavonoids,12 organic acids,9 gallate esterss,5 sesquiterpenoids,3 tannins,4 fatty acids,and 3 amino acids.And 10 components were further confirmed by comparison with the reference substance.MS2 and possible fragmentation pathway of quercetin,neoaconitine,shikimic acid,gallic acid glucose,krillin,dehydroandrolactone,L-proline,and linoleic acid were investigated.Conclusion HPLC-Q-Exactive-MS method could be used to quickly identify the chemical components in Bateri Qiwei Pills,providing reference for its study of pharmacological substances.
作者
杨琳
张谦
李君
YANG Lin;ZHANG Qian;LI Jun(Department of Pharmacy,Hulunbuir Fourth People's Hospital,Hulunbuir 021000,China;College of Pharmacy,Inner Mongolia Medical University,Hohhot 010110,China)
出处
《现代药物与临床》
CAS
2023年第11期2714-2722,共9页
Drugs & Clinic
基金
国家自然科学基金资助项目(82360801)
内蒙古自治区自然科学基金资助项目(2022LHQN08001)
内蒙古自治区高等学校科学研究项目(NJZY22655)。
