UPLC-ESI-Q-TOF-MS^E快速鉴定钩藤中吲哚类生物碱  

Rapid identification of indole alkaloids in Uncaria rhynchophylla by UPLC-ESI-Q-TOF-MS^E

作　　者：布赫 王立乾 唐振球 王斌[1] 王知斌[1] BU Heng;WANG Li-qian;TANG Zhen-qiu;WANG Bin;WANG Zhi-bin(Key Laboratory of Chinese Materia Mediea（Ministry of Education）, Heilongjang Key Laboratory of TCM Pharmacodynamie Material Bases, Heilongjiang University of Chinese Medicine, Harbin 150040, China;College of Pharmacy,Harbin Medical University,Harbin 150081 ,China)

机构地区：[1]黑龙江中医药大学教育部北药基础与应用研究重点实验室黑龙江省中药天然药物药效物质基础研究重点实验室,黑龙江哈尔滨150040 [2]哈尔滨医科大学药物化学与天然药物化学教研室,黑龙江哈尔滨150081

出　　处：《化学工程师》2018年第4期20-24,共5页Chemical Engineer

基　　金：黑龙江中医药大学"优秀创新人才支持计划"科研项目(2012RCD05);黑龙江中医药大学"杰出人才培育"基金项目(2012cj02)

摘　　要：目的通过超高效液相色谱与飞行时间质谱联用技术(UPLC-ESI-Q-TOF-MS^E)快速鉴定和分析钩藤中吲哚类生物碱成分。方法采用色谱柱:HSS T3(100mm×2.1mm,1.8μm,Waters),流动相采用A为0.1%甲酸水溶液,B为乙腈,梯度洗脱。流速为0.4m L·min^(-1),进样量为4μL,正离子MSE扫描模式检测。结果通过对照品数据对照、元素组成分析和碎片结构分析,并结合相关文献,鉴定了9种吲哚类生物碱分别为a.卡丹宾碱、b.二氢卡丹宾碱、c.异去氢钩藤碱、d.柯诺辛碱、e.去氢钩藤碱、f.钩藤碱、g.缝籽嗪甲醚、h.去氢毛钩藤碱、i.毛钩藤碱,并分析其裂解规律。结论 UPLC-ESI-Q-TOF-MS^E可用于快速鉴定钩藤中吲哚类生物碱,为钩藤饮片的质量控制提供了技术支持。Objective The indole alkaloids from the methanol extract of U. rhynchophylla were analyzed and identified rapidly by UPLC-ESI-Q-TOF-MSE. Methods The analysis was performed on an ACQUITY UPLC HSS T3 reverse phase column （100mm ×2.1mm, 1.8μm Waters）. The flow rate was 0.4mL·min^-1, the injection volume was 4 μL. The mobile phase consisted of 0.1% formic acid water and acetonitrile was used for gradient elution. Results The results indicated that nine indole alkaloids （a.Cadambine, b.Dihydrocadambine, c. Isocorynoxeine, d. Corynoxine, e. Corynoxeine, f. Rhynchophylline, g. Geissoschizine methyl ether, h. Hirsuteine, i. Hirsutine.） had been identified by elemental composition analysis, reference substance data comparison, fragment structure analysis and the data of the literature, and further analyzed the fragmentation pathways. Conclusion UPLC-ESI-Q- TOF-MS^E can be used for the rapid identification of indole alkaloids in U. rhynchophylla, and provided technical support for the quality control of U. rhynchophylla.

关 键 词：钩藤 吲哚生物碱 UPLC—ESI—Q—TOF—MS^E 

分 类 号：R284.1[医药卫生—中药学]