摘要
以连翘植物的活性提取物为研究对象,基于不完全分离分析策略,以制备型HPLC技术为分离手段,获取含量呈连续动态变化的系列混合物,运用NMR/LC-MS平行动态谱学方法对提取物中苯乙醇苷类成分进行了同步结构分析研究。采用本方法可获取系列提取物样品中同一成分内在相关且互补的谱学信息,包括保留时间、质荷比(m/z)和化学位移值(δ)等关键数据,结合LC-MS/MS和二维NMR谱分析,成功鉴定出提取物中7种成分的结构,其中包括1个新的苯乙醇苷和1个结构极其罕见的二聚苯乙醇苷生物碱。结果表明,此种谱学分析方法可以简化复杂混合物的分离分析过程,实现结构复杂成分及多组分无需完全分离的快速同步结构鉴定;尤其对于分析极性相近的组分群及常规分离条件下难以获得的微量组分,显示出独特的解析能力。同时,本方法具有从复杂混合物中快速发现及鉴定新的活性成分或先导物的能力,可极大提高分析效率。
Based on an incomplete separation strategy,the crude extract of Forsythia Suspensa was separated into a series of fractions with the concentration of constituent dynamic variation by RP preparative chromatography.NMR/LC-MS parallel dynamic spectroscopic（PDS） method was applied to identify the phenylethanoid glycosides in these fractions.The complementary spectral information of the same individual constituent in the crude extract was simultaneously obtained from the spectra of mixtures,including retention time（Rt）,mass/charge（m/z） and chemical shift（δ）.Seven constituents were identified successfully,including a new phenylethanoid glycoside and a novel Dimeric-2-（4-aminophenyl） ethyl-β-D-glucopyranoside which is the first example of dimeric phenylethanol alkaloid glycoside.The results demonstrated that NMR/LC-MS PDS can be used to identify the constituents with more complicated structures from herbs and their active extracts.Especially,this method is suitable for analysis and identification of minimum-quantity constituents and constituents with similar polarity which are hardly obtained in routine experimental conditions.In addition,this method has the advantage of rapid discovering and identifying new compounds from complex mixtures,which can greatly improve the analytical efficiency.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2011年第3期323-329,共7页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金(No.20775091)资助
关键词
NMR/LC-MS平行动态谱
不完全分离
多组分同步结构鉴定
连翘植物
苯乙醇苷类
Nuclear magnetic resonance/liquid chromatography/mass spectrometry parallel dynamic spectroscopy
Incomplete separation strategy
Simultaneous structural identification in mixture
Forsythia Suspensa
Phenylethanoid glycosides
