摘要
采用二维扩散排序谱(2D-DOSY)和脉冲宽度(PULCON)定量等多种核磁共振(NMR)技术,对具有减肥功效的保健食品中主要成分进行了定性、定量研究。采用布鲁克AvanceⅢ600 MHz超导核磁共振波谱仪,以氘代丙酮为溶剂,对待测物进行了核磁检测。2D-DOSY表明该保健食品中含有3种主要化学成分,结合多种NMR技术对3个化合物进行了结构解析,归属了其所有的NMR谱信号,确定样品的主要成分为邻苯二甲酸二乙酯、褪黑素和奥美拉唑。最后采用PULCON定量技术测得3种成分的绝对含量分别为16.65、5.38、46.35 mg/g。测定结果与HPLC定量结果的对比表明,核磁共振方法能够在无对照品作参比,无需分离的条件下,直接、快速、准确分析保健食品中非目标成分的物质组成和绝对含量。
Qualitative and quantitative determinations on main components in health food were performed by the nuclear magnetic resonance(NMR)techniques such as diffusion-ordered NMR spectroscopy(2D-DOSY)and pulse length based concentration determination(PULCON).In this experiment,Bruker AvanceⅢ600 MHz was applied,with acetone-d 6 as solvent.2D-DOSY spectra demonstrated that the sample contained three compounds.1H-1H correlation spectroscopy(COSY)and total correlation(TOCSY),1H-13 C heteronuclear single quantum coherence spectroscopy(HSQC)and 1H-13 C heteronuclear multiple bond correlation(HMBC)were used to assign the chemical shifts of the compounds,which were finally determined to be diethyl phthalate,melatonin and omeprazole.Finally,a quantitative PULCON method was developed to determine the contents of by-products,and the contents of the three compounds were 16.65,5.38,46.35 mg/g,respectively.The results indicated that the NMR spectroscopy,compared with HPLC method,is a more direct and rapid method for analysis on the structures and contents of non-target compounds in health food with no need of standard reference and separation.
作者
李玮
耿健强
涂光忠
LI Wei;GENG Jian-qiang;TU Guang-zhong(Beijing Municipal Center for Food Safety Monitoring and Risk Assessment,Beijing 100094,China;Beijing Institute of Microchemistry,Beijing 100091,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2018年第3期288-293,共6页
Journal of Instrumental Analysis
基金
北京市科技计划(Z151100001215006
D16110500210000)
关键词
核磁共振
扩散排序
脉冲宽度定量
保健食品
非目标成分
NMR
diffusion-ordered NMR spectroscopy(DOSY)
pulse length based concentration determination(PULCON)
health food
non-target component
