| 土荆皮中二萜类化合物的HPLC-ESI/MS~n鉴定(英文) |
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| 引用本文： | Liu P,Sun JH,Xu M,Guo H,Guo HZ,Kang J,Han J,Wang BR,Guo DA. 土荆皮中二萜类化合物的HPLC-ESI/MS~n鉴定(英文)[J]. 药学学报, 2011, 46(2): 213-220 |
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| 作者姓名： | Liu P Sun JH Xu M Guo H Guo HZ Kang J Han J Wang BR Guo DA |
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| 作者单位： | 北京大学医学部药学院天然药物学系;国家知识产权局;北京市药品检验所; |
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| 基金项目： | supported by the National High Technology Research and Development Program of China(Grant No.2003AA2Z2030); program for Changjiang Scholar and Innovative Team in University(Grant No.985-2-063-112) |
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| 摘 要： | 使用高效液相色谱-多级质谱法(HPLC-ESI/MSn)研究了土荆皮二萜的ESI/MSn裂解行为,并对土荆皮中的二萜类化合物进行了定性分析。土荆皮二萜的特征裂解是内酯环和C4-O键的断裂。此外,C-18、C-7和C-8位取代基的离去在多级质谱(MSn,n=3～4)中也可观察到。对于C-4位乙酰氧基取代的二萜,[M+Na-60]+和[M-H-104]-分别是正、负离子模式下二级质谱的基峰。对于C-4位羟基取代的二萜,[M+Na-44]+和[M-H-62]-分别是正、负离子模式下二级质谱的基峰。对于C-18位葡萄糖苷化或酯化的二萜,[M+Na-44]+是正离子模式下二级质谱的基峰。利用上述裂解规律,使用LC-MS方法在正离子模式下鉴定了土荆皮甲醇-水(6∶4)提取物中的二萜类化合物,共有9个二萜被鉴定或初步推测,其中一个是首次报道的化合物。所述方法可用于土荆皮的灵敏快速定性分析。
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| 关 键 词： | 土荆皮 二萜 质量控制 定性分析 高效液相色谱-多级质谱 裂解 |
Characterization of diterpenoids in the bark of Pseudolarix kaempferi by HPLC-ESI/MSn |
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| Liu Peng,Sun Jiang-hao,Xu Man,Guo Hui,Guo Hong-zhu,Kang Jie,Han Jian,Wang Bao-rong,Guo De-an. Characterization of diterpenoids in the bark of Pseudolarix kaempferi by HPLC-ESI/MSn[J]. Acta pharmaceutica Sinica, 2011, 46(2): 213-220 |
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| Authors: | Liu Peng Sun Jiang-hao Xu Man Guo Hui Guo Hong-zhu Kang Jie Han Jian Wang Bao-rong Guo De-an |
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| Affiliation: | LIU Peng1,2,SUN Jiang-hao1,XU Man1,GUO Hui1,GUO Hong-zhu1,3,KANG Jie1,HAN Jian1,WANG Bao-rong1,GUO De-an1(1.Department of Natural Medicines,School of Pharmaceutical Sciences,Peking University Health Science Center,Beijing 100083,China,2.State Intellectual Property Office of The P.R.C.,Beijing 100088,3.Beijing Institute for Drug Control,Beijing 100035,China) |
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| Abstract: | Fragmentation behavior of diterpenoids was investigated by ESI/MSn and the qualitative analysis of diterpenoids in the bark of Pseudolarix kaempferi was performed using high-performance liquid chromatography/ multi-stage mass spectrometry(HPLC-ESI/MSn).The characteristic fragmentation behaviors of the diterpenoids are the cleavages of the lactone ring and C4-O bond.Furthermore,the eliminations of substituent groups at C-18,C-7 and C-8 can also be observed in the MSn(n=3-4) spectra.For C-4 acetoxy subsititue... |
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| Keywords: | Pseudolarix kaempferi diterpenoid quality control qualitative analysis HPLC-ESI/MSn fragmentation |
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