摘要
以核桃青皮粉为原料,75%的甲醇为提取剂,超声波微波萃取仪辅助多级萃取后,经薄层层析获得醌类化合物单体;通过光谱、色谱与质谱检测分析,并结合其旋光度和熔点,确认其化合物。结果表明,甲醇-水(3∶1)为提取剂,在超声波恒定的条件下,超声波微波萃取仪优化方案为温度40,45,50℃;微波频率100,200,300 MHz;超声波功率850,900,800 W;模式15∶10,电机转速900 r/min;在展开剂为正己烷∶乙酸乙酯∶乙醇=8∶1∶1下,供试样液的斑点与胡桃醌对照品有大致相同的Rf值;该单体含有苯环、羟基、羰基,与醌类化合物的官能团一致,其相对分子质量在碎片丢失范围内;熔点为156℃,旋光度和比旋光度分别为57.166,1.744。该方法可行性高、简便可靠,适用于从核桃青皮中进行物质的制备分离。
Walnut green peel powder was used as raw material,75%methanol was used as extraction agent,and ultrasonic-microwave assisted multistage extraction was carried out.Quinone monomers were obtained by TLC.The compounds were identified by spectroscopic,chromatographic and mass spectrometry,combined with their optical rotation and melting point.The results showed that methanol-water(3∶1)was used as extraction agent.Under constant ultrasonic conditions,the optimized scheme of ultrasonic microwave extraction instrument was as follows:temperature was 40,45,50℃,microwave power was 100,200,300 MHz,ultrasonic frequency was 850,900,800 W,mode was 15∶10,motor speed was 900 r/min.When the developing agent was n-hexane∶ethyl acetate∶ethanol=8∶1∶1,the spots of the sample solution had roughly the same Rf value as that of the guanone control.The monomer contains benzene ring,hydroxyl group and carbonyl group,which was consistent with the functional groups of quinones,and its relative molecular weight was within the range of debris loss.The melting point is 156℃,and the rotation and specific rotation were 57.166,1.744,respectively.The method is feasible,simple and reliable,and suitable for the preparation and separation of the substances from walnut peel.
作者
杜京旗
陈娇娇
杨卫民
DU Jingqi;CHEN Jiaojiao;YANG Weimin(Provincial and Local Joint Cultivation Base,Shanxi Key Laboratory of Phytochemistry in Lvliang,Shanxi Engineering Research Center of Plant Functional Composition,Lvliang University,Lvliang,Shanxi 033001,China)
出处
《农产品加工》
2021年第12期56-59,共4页
Farm Products Processing
基金
山西省重点实验室计划项目(201805D111012)
山西省重点研发计划项目(201803D221011-6)
吕梁市引进高层次科技人才专业科技创新平台建设项目(2018-21-11)
山西省“1331工程”工程(技术)研究中心建设计划项目(PT20181206)。
关键词
核桃青皮
薄层层析
醌类化合物
红外光谱仪
质谱仪
walnut green peel
thin layer chromatography(b)
quinone compounds
infrared spectrometer
mass spectrometer
作者简介
杜京旗(1984-),男,在读博士,讲师,研究方向为植物生理生态学;通讯作者:杨卫民(1960-),男,本科,教授,研究方向为特色植物资源研究与利用。
