薄层色谱—表面增强拉曼光谱法快速检测改善睡眠类保健食品的主要成分及其光谱表征  

Rapid on-site thin layer chromatography-surface enhanced Raman spectroscopy detection of main ingredient in health-care food and its spectral characterization

作　　者：李静辉[1] 刘吉成[1] 马德志[1] 李慧 孔婉莹 张可勇[1] LI Jing-hui;LIU Ji-cheng;MA De-zhi;LI Hui;KONG Wan-ying;ZHANG Ke-yong(Qiqihar Medical University,Heilongjiang Qiqihar 161006,China)

机构地区：[1]齐齐哈尔医学院,黑龙江齐齐哈尔161006

出　　处：《中国食品卫生杂志》2018年第4期376-382,共7页Chinese Journal of Food Hygiene

基　　金：国家自然科学基金项目(81573660);黑龙江省齐齐哈尔市科学技术计划项目(SFGG-201541);齐齐哈尔医学院院内基金项目(QY2016GJ-02)

摘　　要：目的建立薄层色谱(TLC)与表面增强拉曼光谱(SERS)联用技术对改善睡眠类保健食品的主要成分(褪黑素、维生素B_6)的快速检测新方法。方法以环己烷-乙酸乙酯-乙醇(5∶3.5∶2,V/V)为展开剂,利用TLC将改善睡眠类保健食品中主要成分与保健食品基质初步分离,在UV_(254nm)下检测定位;以780 nm激光为激发波长,水相银胶溶液为表面增强剂,采用SERS法对TLC上的微量成分进行原位定性检测。通过模拟阳性样品试验,考察保健食品基质对褪黑素、维生素B_6的TLC-SERS的影响,并考察褪黑素及维生素B_6的检出限,并随机对市售4种改善睡眠类保健食品进行检测。结果褪黑素、维生素B_6的TLC-SERS与相应对照品的拉曼光谱特征峰存在明显相关性;保健食品的基质对褪黑素和维生素B_6的检测不存在干扰;褪黑素和维生素B_6的检出限为10、5μg。市售改善睡眠类保健食品主要成分的TLC-SERS与褪黑素或维生素B_6基本相同。结论本法准确、灵敏、快速、简单,为检测混合样品等复杂体系主要成分的定性鉴别检测提供一种有效方法。Objective A novel facile method for on-site detection of main ingredient（ e. g. melatonin,vitamin B_6） in health-care food for promoting sleep using thin layer chromatography（ TLC） combined with surface enhanced Raman spectroscopy（ SERS） was reported. Methods Firstly,main components were separated with substrate in health-care food by TLC initially,the mobile phase was cyclohexane-ethyl acetate-ethanol（ 5 ∶ 3. 5 ∶ 2,V/V）; detected and located by UV under254 nm. Then trace substances were qualitatively detected by SERS,the excitation wavelength was 780 nm,and the surface enhancer was aqueous phase silver sol. The effect of matrix on the melatonin and vitamin B_6 was investigated by TLC-SERS in the positive experiment,and the detection limits of melatonin and vitamin B_6 were also investigated. In addition,four commercially available health-care food products to improve sleep were tested,randomly. Results The characteristic peaks of Raman spectra of melatonin and vitamin B_6 obtained by TLC-SERS method were nearly consistent with the reference substance. The matrix of health-care food to add ingredients was no interference on the target substance. The limit of mole tection（ LOD） of melatonin and vitamin B_6 were 10 and 5 μg. The TLC-SERS of main components was the same with melatonin or vitamin B_6 substantially. Conclusion This method was accurate,sensitive,fast,and simple. It provides an effective method for the qualitative identification and detection of complex components such as mixed samples.

关 键 词：薄层色谱 表面增强拉曼光谱 拉曼光谱 光谱法 褪黑素 维生素B_6 改善睡眠类保健食品 

分 类 号：R155[医药卫生—营养与食品卫生学]