摘要
使用高压液相色谱和荧光检测器对咖啡因样品进行分离和荧光检测,经过优化确定采用220 nm为激发波长、400 nm为发射波长进行检测,建立了相对于咖啡因的荧光物质含量的定量方法,并对不同咖啡因样品进行分析。研究发现,粗品咖啡因中荧光物质主要有6种,合格成品咖啡因中荧光物质剩余4种,确定保留时间为17.29 min的物质(简称物质3)为导致产品荧光指标不合格的主要物质。采用工业上常用的高锰酸钾氧化、连二亚硫酸钠还原、活性炭吸附和重结晶咖啡因精制方法对回收的一浓品咖啡因进行了处理。结果表明,重结晶能够有效脱除物质3,脱除效率为89.5%,其他方法都不能有效去除物质3且呈现出不同的影响趋势。
High pressure liquid chromatography and fluorescence detector are employed to separate and detect the fluorescence substances present in synthetic caffeine samples.After optimization, the excitation wavelength and emission wavelength are determined to be 220 nm and 400 nm, respectively.A quantitative method for analyzing the content of fluorescent substances relative to caffeine is established, and used to analyze different caffeine samples.It is found through research that there are 6 kinds of fluorescent substances in crude caffeine and 4 kinds in qualified finished caffeine.It is determined that the substance with retention time of 17.29 min(hereafter referred as “substance 3”) is the main factor leading to the failure of fluorescent test.Several common industrial processing methods such as KMnO4oxidation, Na2S2O4reduction, activated carbon adsorption and recrystallization are respectively used to treat with a recovered caffeine sample, and their effects on content of substance 3 are given.It is verified that recrystallization can effectively remove substance 3 with a removal rate of 89.5%.Other methods cannot effectively remove substance 3 and show different impact trends.
作者
岳金彩
李晓阳
周波
郑世清
YUE Jin-cai;LI Xiao-yang;ZHOU Bo;ZHENG Shi-qing(College of Chemical Engineering,Qingdao University of Science and Technology,Qingdao 266042,China;Qingdao Yinke Hengyuan Chemical Process Information Technology Co.,Ltd.,Qingdao 266042,China)
出处
《现代化工》
CAS
CSCD
北大核心
2022年第12期269-272,共4页
Modern Chemical Industry
基金
山东省自然科学基金项目(ZR2020MB145)。
关键词
咖啡因
荧光
重结晶
精制
caffeine
fluorescence
recrystallization
refine