天然产物研究与开发 ›› 2016, Vol. 28 ›› Issue (11): 1758-1763.doi: 10.16333/j.1001-6880.2016.11.013

• 研究简报 • 上一篇    下一篇

基于HPLC-ESI-TOF/MS法分析测定乌天麻和红天麻中化学成分的研究

李云1,王志伟2,耿岩玲2,周洪雷1,刘大会3*,王晓1,2*   

  1. 1 山东中医药大学药学院;2山东省中药质量控制技术重点实验室,山东省分析测试中心,济南 250014;3 云南省农业科学院药用植物研究所,昆明 650231
  • 出版日期:2016-11-30 发布日期:2017-03-30

Determination of Chemical Constituents in Gastrodia elata f. Glauca and Gastrodia elata f.Elata by HPLC-ESI-TOF/MS

LI Yun1,WANG Zhi-wei2,GENG Yan-ling2,ZHOU Hong-lei1,LIU Da-hui3*,WANG Xiao1,2*   

  1. 1 College of Pharmacy,Shandong University of Traditional Chinese Medicine,Jinan 250014,China;2Shandong Analysis and Test Center,Key Laboratory of TCM Quality Control Technology,Jinan 250014,China; 3Medicinal Plant Research Institute of Yunnan Academy of Agricultural Sciences,Kunming 650231,China
  • Online:2016-11-30 Published:2017-03-30

摘要: 建立高效液相色谱-电喷雾飞行时间质谱(HPLC-ESI-TOF/MS)联用技术用于指认乌天麻和红天麻中的化学成分,并对天麻素、对羟基苯甲醇、对羟基苯甲醛、腺苷、巴利森苷 A、4,4′-二羟基二苄基醚6 种成分进行含量测定。采用Agilent 1120高效液相系统,YMC-PEAK ODS-A column(250 mm × 4.6 mm,5 μm)色谱柱,流动相为0.1%甲酸水溶液(A)-甲醇溶液(B),梯度洗脱:0~5 min,5% B;5~65 min,5%~40% B;65~80 min,40%~100% B;分析时间80 min;体积流量1 mL/min;柱温25 ℃;进样量50 μL。最终指认了天麻提取物中的15种成分,其中天麻素、对羟基苯甲醇、对羟基苯甲醛、腺苷、巴利森苷 A、4,4′-二羟基二苄基醚6种成分在线性范围内均具有良好的线性关系(r≥0.9991);平均回收率在 94.90%~99.81%之间,RSD<2.40%。在不同品种的天麻饮片中,6种成分的量存在差异,红天麻各成分含量稍高于乌天麻,一级乌天麻各成分含量高于二级乌天麻。同一品种天麻中,巴利森苷类成分含量较高,腺苷和4,4′-二羟基二苄基醚含量均较低。建立的HPLC测定方法分离效果与重复性好、快速、简便,为天麻饮片的质量控制提供参考。

关键词: 天麻, HPLC-ESI-TOF/MS, 天麻素, 对羟基苯甲醇, 巴利森苷A, 含量测定

Abstract: To establish a high performance liquid chromatography-electrospray time-of-flight mass spectrometry (HPLC-ESI-TOF/MS) method for the identification of chemical ingredients in Gastrodia elata Blume,and to determine the content of gastrodin,p-hydroxybenzyl alcohol,p-hydroxybenz aldehyde,adenosine,parishin A and 4,4′-dihydroxydibenzyl ether.The analysis was performed on an Agilent 1120 system using a YMC-PEAK ODS-A column (250 mm × 4.6 mm,5 μm).The 6 components were separated in 80 min with gradient mobile phase consisting of 0.1% CH3COOH-H2O (A) and CH3OH (B):0-5 min,5% B;5-65 min,5%-40% B;65-80 min,40%-100% B.Volume flow rate was 1 mL/min.The temperature was set at 25 ℃,and the injection volume was 50 μL.Ultimately,15 ingredients in G.elata was identified,in which the content of 6 components were determined by the developed HPLC-ESI-TOF/MS method.The results showed good linear relationship (r≥0.9991),the average recoveries were in the range of 94.90%-99.81% with RSD%<2.40.There were differences in the amounts of 6 components in different varieties of G.elata. The contents of 6 components in G.elata f.Elata is slightly higher than those in G.elata f.Glauca.In the same variety,the amounts of the 6 compounds in first grade herb were higher than in second grade.The developed HPLC-ESI-TOF/MS method was simple,sensitive and had good repeatability.

Key words: Gastrodia elata, HPLC-ESI-TOF/MS, gastrodin, p-hydroxybenzyl alcohol, parishin A, determination of content

中图分类号: 

R917