TONG Xiao-lin, NIE Ying-lan, MA Yan-yan, et al. LC-MSAnalysis of Chemical Constituents of Fritillaria Ussuriensis Bulbus Water Solution[J]. Chinese journal of experimental traditional medical formulae, 2016, 22(21): 45-49.
DOI:
TONG Xiao-lin, NIE Ying-lan, MA Yan-yan, et al. LC-MSAnalysis of Chemical Constituents of Fritillaria Ussuriensis Bulbus Water Solution[J]. Chinese journal of experimental traditional medical formulae, 2016, 22(21): 45-49. DOI: 10.13422/j.cnki.syfjx.2016210045.
LC-MSAnalysis of Chemical Constituents of Fritillaria Ussuriensis Bulbus Water Solution
目的:为深入研究平贝母水煎液内的化学成分,采用水煎煮法对平贝母鳞茎进行提取,运用液相色谱-离子肼质谱联用仪(LC-MSn)建立一种方法对平贝母水煎液中的化学成分进行分析。方法:通过LC-MSn联用技术判定平贝母水煎液内成分,采用Agilent ZORBAX Extend-C18色谱柱(2.1 mm×50 mm 1.8 μm),乙腈-0.1%氨水梯度洗脱模式,ESI离子源,正离子模式下采集数据。根据平贝母水煎液内成分和对照品之间的总离子流图、多级质谱图、质谱碎片信息进行对比以及成分标准质谱裂解规律测定平贝母水煎液中的化学成分。结果:从平贝母水煎液中共分离出22个峰,鉴别出19个生物碱成分,发现3个未知生物碱成分。结论:实验结果表明,LC-MSn方法适用于平贝母中生物碱成分的常规分析,可进一步提高对平贝母药效物质基础的认识,为平贝母的化学成分研究和质量控制建立了实验和理论基础。
Abstract
Objective: To study the chemical constituents in Fritillaria Ussuriensis Bulbus water solution
extract Fritillaria Ussuriensis Bulbus by the method of water solution
and establish LC-ESI-TRAP-MS (LC-MSn) method to analyze the chemical components in Fritillaria Ussuriensis Bulbus water solution. Method: LC-MSn method was used to determine the chemical components in Fritillaria Ussuriensis Bulbus on Agilent ZORBAX Extend-C18 column (2.1 mm×50 mm 1.8 μm)
with acetonitrile-0.1%ammonia as the mobile phase for gradient elution. Data were collected with posi tive ESI source. Structures of the components were elucidated by comparing the total ion chromatogram
multi-stage mass spectrogram
and mass spectrometry fragment information between Fritillaria Ussuriensis Bulbus water solution and control products and by referring to the compound standard mass spectrometry fragmentation rules. Result: The 22 peaks were found in this study; 19 alkaloid components were identified; and 3 unknown alkaloid components were found from Fritillaria Ussuriensis Bulbus water solution. Conclusion: LC-MSn method is suitable for the routine analysis of alkaloid components in Fritillaria Ussuriensis Bulbus and also can help to improve the understanding of its pharmacodynamic action
providing experimental and theoretical basis for the study of chemical components and quality control of Fritillaria Ussuriensis Bulbus.
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