UPLC-ESI-MS/MS法测定苗药隔山消中8个成分含量  

Determination of eight constituents in radix cynanchi of miao medicine by UPLC-ESI-MS/MS

作　　者：秦兰 孙佳[3] 刘春花[1] 陆苑[3] 潘洁[1] 李勇军[1] 王永林[3] 林昌虎[1] QIN Lan;SUN Jia;LIU Chunhua;LU Yuan;PAN Jie;LI Yongjun;WANG Yonglin;LIN Changhu(State Key Laboratory of Functions and Applications of Medicinal Plants&Engineering Research Center for the Development and Application of Ethnic Medicine and TCM of Ministry of Education,Guizhou Medical University,Guiyang 550004,Guizhou,China;School of Pharmacy,Guizhou Medical University,Guiyang 550004,Guizhou,China;Guizhou Provincial Key Laboratory of Pharmaceutics,Guizhou Medical University,Guiyang 550004,Guizhou,China)

机构地区：[1]贵州医科大学民族药与中药开发应用教育部工程研究中心&省部共建药用植物功效与利用国家重点实验室,贵州贵阳550004 [2]贵州医科大学药学院,贵州贵阳550004 [3]贵州医科大学贵州省药物制剂重点实验室,贵州贵阳550004

出　　处：《贵州医科大学学报》2021年第8期886-892,共7页Journal of Guizhou Medical University

基　　金：国家自然科学基金(81760700,U1812403);中央引导地方科技专项项目[黔科中引地(2018)4006];博士科研启动基金[校博合J字(2020)013]。

摘　　要：目的建立超高效液相色谱-电喷雾电离-串联质谱法(UPLC-ESI-MS/MS)检测隔山消中告达亭、松脂素、白首乌二苯酮、阿魏酸、没食子酸、东莨菪内酯、丁香酸及绿原酸8个成分含量的标准。方法选取13批不同产地隔山消,采用UPLC-ESI-MS/MS法,以ACQUITY UPLC BEH C 18(2.1 mm×100 mm,1.7μm)为色谱柱,0.1%甲酸水溶液-0.1%甲酸乙腈溶液为流动相、梯度洗脱、流速0.35 mL/min、柱温40℃,采用电喷雾离子源(ESI)和多反应离子监测(MRM)模式检测其中告达亭、松脂素、白首乌二苯酮、阿魏酸、没食子酸、东莨菪内酯、丁香酸及绿原酸的含量。结果告达亭、松脂素、白首乌二苯酮、阿魏酸、没食子酸、东莨菪内酯、丁香酸及绿原酸的质量浓度分别于1.860~119.048μg/L、148.950~4766.400μg/L、186.012~47619.045μg/L、5.813~11904.760μg/L、2.325~148.809μg/L、3.720~952.380μg/L、37.202~4761.900μg/L及3.720~1904.760μg/L范围内与峰面积呈良好线性关系,r>0.9990,平均加样回收率范围95.247%~102.432%;13批样品中告达亭、松脂素、白首乌二苯酮、阿魏酸、没食子酸、东莨菪内酯、丁香酸及绿原酸的含量测定结果分别为0.443~2.958μg/g、6.794~22.436μg/g、33.584~649.745μg/g、1.828~55.290μg/g、0.102~0.304μg/g、0.525~5.213μg/g、2.052~7.757μg/g及8.042~31.608μg/g;不同批次各成分的含量差异较大,其中白首乌二苯酮含量最高,松脂素、阿魏酸和绿原酸的含量相对较高,其余成分含量较低。结论UPLC-ESI-MS/MS法可作为隔山消药材质量控制的检测方法。Objective To establish the determination standard of 8 components of caudatin,pinoresinol,beishouwubenzophenone,ferulic acid,gallic acid,scopoletin,syringic acid and chlorogenic acid in radix cynanchi by ultra-high-performance liquid chromatography electrospray ionization tandem mass spectrometry.Methods Contents of caudatin,pinoresinol,beishouwubenzophenone,ferulic acid,gallic acid,scopoletin,syringic acid and chlorogenic acid in 13 batches of radix cynanchi from different areas were tested by using UPLC-ESI-MS/MS.The chromatographic separation was performed on an ACQUITY UPLC BEH C 18(2.1 mm×100 mm,1.7μm)with a mobile phase consisting of 0.1%formic acid acetonitrile-0.1%formic acid at the flow rate of 0.35 mL/min,and the column temperature was 40℃.Electrospray ionization source(ESI)was used combined with multiple reaction monitoring(MRM)mode mass spectral acquisition.Results The linear ranges for caudatin,pinoresinol,beishouwubenzophenone,ferulic acid,gallic acid,scopoletin,syringic acid,chlorogenic acid were 1.860-119.048μg/L,148.950-4766.400μg/L,186.012-47619.045μg/L,5.813-11904.760μg/L,2.325-148.809μg/L,3.720-952.380μg/L,37.202-4761.900μg/L and 3.720-1904.760μg/L showed good respectively(r>0.9990),whose average recoveries were 96.845%-102.432%.The contents of caudatin,pinoresinol,beishouwubenzophenone,ferulic acid,gallic acid,scopoletin,syringic acid,chlorogenic acid in 13 batches of radix cynanchi of miao medicine were 0.443-2.958μg/g,6.794-22.436μg/g,33.584-649.745μg/g,1.828-55.290μg/g,0.102-0.304μg/g,0.525-5.213μg/g,2.052-7.757μg/g and 8.042-31.608μg/g,respectively.There were great differences in the contents of various components among different batches,in which the content of beishouwubenzophenone was the highest,the contents of pinoresinol,ferulic acid and chlorogenic acid were relatively high,and the contents of other components were lower.Conclusion The UPLC-ESI-MS/MS method can provide a reference for the quality control of radix cynanchi.

关 键 词：质量控制 隔山消 多反应离子监测模式 含量测定 超高效液相色谱-电喷雾串联质谱联用 白首乌二苯酮 

分 类 号：R917[医药卫生—药物分析学]