液相色谱-多级质谱联用法分析核桃壳提取物化学成分

Analysis of the chemical constituents of walnut shell extract by liquid chromatography-multistage mass spectrometry

为了更好地提升核桃壳的技术附加值和工业化应用,采用了液相色谱-多级质谱联用方法分析核桃壳提取物化学成分.以核桃壳为原料,将粉碎的核桃壳样品用二氯甲烷-甲醇-水混合溶剂进行水浴超声处理.将上清液旋蒸氮吹近干后复溶得到的棕色液体经膜过滤后稀释,经仪器分离分析,得到提取物成分的总离子流图.在对应峰处找到母离子,对5个峰值比较明显的母离子进行化合物初步推测.再对母离子进行MS2碎片扫描得到子离子碎片,根据化合物的多级质谱信息,对其结构分析进而确定核桃壳中含有5-羟甲基-2-呋喃甲醛、十八烷酸、δ-生育酚.该方法有利于核桃壳成分的快速鉴定,可为其成分进一步研究提供基础,促进核桃壳的高效综合开发利用.

In order to improve the technological added value and the industrial application of walnut shell,the method of liquid chromatography mass spectrometry was established to analyze the chemical components of walnut shell extract.Using walnut shell as raw material,the crushed walnut shell samples were treated by water bath ultrasonic treatment with CH2Cl2-CH3OH-H2O.Supernatant was extracted,evaporated and blown to near dry by nitrogen flow,which was re-dissolved to obtain brown liquid.The brown liquid was diluted with the filter membrane.After the separation and analysis with the instrument,the total ion flow diagram of the extract components was obtained.The parent ions were found at the corresponding peaks,and the five parent ions with obvious peaks were preliminarily speculated.Then the parent ion was scanned by MS2 fragment to obtain the daughter ion fragments.According to the multistage mass spectrometry information of the compound,the structure of the walnut shell was analyzed and the contents of 5-hydroxymethyl-2-furan formaldehyde,stearic acid andδ-tocopherol were determined.This method is conducive to the rapid identification of walnut shell components,which can provide a basis for further study of its components,and promote the efficient and comprehensive development and utilization of walnut shell.