油菜蜂花粉中一种核苷类成分的分离

Separation of a Nucleoside Analogue from Rape Bee Pollen

为了研究油菜蜂花粉中核苷类成分的组成,本实验采用15%乙醇进行超声提取,结合薄层色谱法(thin layerchromatography,TLC)分析(展开剂为氯仿-甲醇-氨水,体积比为6.5:8.0:1.5),再经D101大孔吸附树脂柱层析(洗脱剂为5%乙醇)、水饱和正丁醇萃取及高效液相色谱法(high-performance liquid chromatography,HPLC)分离纯化,最终分离得到单一化合物,通过液相色谱-四极杆-飞行时间串联质谱法(liquid chromatography-quadrupole-time offlight mass spectrometer,LC-Q-TOF)对其相对分子质量、不饱和度、同位素匹配度、相似度进行分析,通过HPLC法比较样品与标准品的保留时间、紫外光谱图比对,确认该化合物为腺嘌呤(adenine)。

In order to explore the nucleoside composition of rape bee pollen,the sample was subjected to extraction with 15% aqueous ethanol under the assistance of ultrasonic,TLC analysis using chloroform-methanol-ammonia（6.5：8.0：1.5,V/V） as the development solvent,chromatographic separation on D101 type macroporous adsorption resin column using 5% aqueous ethanol as the elution solvent,water saturated butanol extraction and high-performance liquid chromatographic（HPLC） purification and as a result,a single compound was obtained.The compound was identified as adenine by liquid chromatography-quadrupole-time of flight mass spectrometer（LC-Q-TOF） according to the data of accurate mass,double bond equivalent（DBE）,spacing match and similarity score and by comparison of its retention time and UV spectrum with those of the reference substance.