TLC-SERS法快速检测改善睡眠类保健食品中四种化学成分

摘要

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中四种非法添加化学成分(三唑仑、艾司唑仑、氯硝西泮及奥沙西泮)的快速检测新方法.以环己烷-乙酸乙酯-乙醇(5:3.5:2)为展开剂,利用 TLC 将添加成分与保健食品基质初步分离,在UV254 nm下检测定位;以780 nm激光为激发波长,水相银溶胶为表面增强剂,采用SERS法对TLC上的微量添加成分定性检测.通过模拟阳性样品实验,考察保健食品基质对添加成分TLC-SERS的影响,并考察四种化学成分的检测限.建立了改善睡眠类保健品中非法添加四种化学成分的TLC-SERS检测方法.四种添加成分的 TLC-SERS与相应对照品的拉曼光谱特征峰存在明显相关性;保健食品的基质对添加成分的检测几乎没有干扰;四种化学成分的检测限为1~4 μg.最后,对市售五种改善睡眠类保健食品进行检测,均不存在非法添加情况.该研究利用T LC与SERS相结合的方法应用于改善睡眠类保健食品中掺杂化学成分的快速检测,并获得了镇静安眠类共四种化药的TLC-SERS谱,建立了改善睡眠类保健食品中非法添加三唑仑等四种化药的检测方法;该法专属、灵敏、快速、简单,并且没有显著的检测时间限制,为改善睡眠类保健食品中掺杂化学成分的现场检测方法研究提供新的参考依据.%A novel facile method for on-site detection of sleep problems chemicals(e.g.triazolam,estazolam,clonazepam and oxazepam)adulterated in health-care food for promoting sleep using thin layer chromatography(TLC)combined with surface en-hanced Raman spectroscopy(SERS)was reported in the present paper.Firstly,chemical drugs added in simulation of positive drugs were separated with substrate in health-care food by TLC initially,mobile phase was cyclohexane-ethyl acetate-ethanol (5:3.5:2);detected and located by UV under 254 nm.Then trace substances were qualitative detected by SERS,excitation wavelength was 780 nm,surface enhancer was aqueous phase silver sol.The effect of matrix on the addition of health-care food was investigated by TLC-SERS in the positive experiment,and the detection limits of the 4 kinds of chemical components were also investigated.TLC-SERS detection method for 4 kinds of chemical components,which were illegally added in sleep health care products,was established.The characteristic peaks of Raman spectra of the chemical drugs added into health-care food ob-tained by TLC-SERS method were nearly consistent with the reference substance.TLC-SERS of matrix of health-care food to add ingredients was almost no interference.The LOD of 4 kinds of chemical components was from 1 to 4 μg.In addition,com-mercially available five kinds of Chinese medicine and health-care food for improving sleep were tested,randomly;there was no illegal substance added in the case.In this study,TLC-SERS method is applied in rapid testing of health-care food adulteration for the first time,with obtaining some ideal results,such as SERS spectra of 4 kinds of sedative hypnotics chemical drugs,as well as TLC-SERS detection methods for 4 frequently adulterated sedative hypnotics chemical drugs.TLC-SERS method is spe-cific,sensitive,rapid,and without significant detection time constraints,would have good prospects in on-site detection of chemicals for doping in health-care food.