天麻中对羟基苯类化合物的高效液相色谱-质谱研究

Study of p-Hydroxyphenylic Compounds in Gastrodia Elata Blume by High Performance Liquid Chromatography-Electrospray -Mass Spectrometry

天麻中对羟基苯类化合物的 (ESI(- ) )一级质谱图中除分子离子峰 [M - 1]外 ,还可见明显的[M - 1+2 0 ]和 [2M - 1]峰 ,由此规律可方便确证未知同类样品的分子离子峰。由二级质谱 (ESI MS MS)的特征碎片离子 93、10 5和 10 7等 ,结合紫外光谱及核磁结果确定了 3个不纯样品中主要成分的结构 ,同时初步确定了两个同类杂质的结构。

To identify the main, components from three impure samples in Gastrodia elata blume, a method of high performance liquid chromatography-electrospray-mass spectrometry-mass spectrometry (HPLC/ESI/MS/MS) was used. First, three identified p-hydroxyphenylic compounds were analyzed by HPLC/ESI/MS. Molecular ions [M - 1] and other two characteristic ions [M - 1 + 20] and [2M - 1] were clearly observed in their negative electrospray-mass (ESI(-)) spectra. According to this rule, the molecular,ions from unknown p-hydroxyphenylic compounds can be easily identified by using the same method. Secondly, Combining characteristic fragmentary ions obtained by MS/MS spectra and other structural information such as chemical reaction, nuclear magnetic resonance (NMR) and ultraviolet spectra (UV), five compounds from three impure samples in Gastrodia elata Blume were successfully clarified in which three were the main components from the samples and two others were trace components. So, the method of HPLC/ESI/MS/MS may be used to identify the structure of main components from impure samples, it can be also used as a guide method for separating.