TLC-SERS同时检测降压类保健食品中五种沙坦类违禁添加成分  

Simultaneous Determination of Five Banned Sartan Compounds inAntihypertensive Health Food Using Thin-Layer ChromatographyCombined With Surface-Enhanced Raman Spectroscopy(TLC-SERS)

作　　者：黄丽俊 庄顺钱 冯永巍 杨方威 孙震 谢云飞[2] 薛庆海 HUANG Li-jun;ZHUANG Shun-qian;FENG Yong-wei;YANG Fang-wei;SUN Zhen;XIE Yun-fei;XUE Qing-hai(Wuxi Food Safety Inspection and Test Center,Wuxi 214412,China;School of Food Science and Technology,Jiangnan University,Wuxi 214122,China)

机构地区：[1]无锡市食品安全检验检测中心,江苏无锡214412 [2]江南大学食品学院,江苏无锡214122

出　　处：《光谱学与光谱分析》2024年第5期1354-1363,共10页Spectroscopy and Spectral Analysis

基　　金：国家“十四五”重点研发计划项目(2018YFC1602303);江苏省市场监督管理局科技计划项目(KJ21125006)资助。

摘　　要：由于人们不健康的饮食结构和生活作息习惯以及人口老龄化等因素,高血压等慢性病发病率逐渐增高,降压类保健食品逐渐受到人们青睐。但是市场中存在不良商家为了提高保健食品的功效,向保健食品中非法添加降压药,尤其是沙坦类降压药的现象。建立了一种薄层色谱层析技术(TLC)与表面增强拉曼光谱(SERS)联用方法,对降压类保健食品中五种可能添加的沙坦类违禁成分(奥美沙坦酯、厄贝沙坦、氯沙坦钾、替米沙坦、缬沙坦)进行同步检测。对五种药物的SERS检测最佳条件进行探究,并通过比较不同成分及配比的TLC展开剂对于五种药物的分离效果,经过大量配方试验后成功得到环己烷-乙酸乙酯-甲醇-冰醋酸=53∶35∶12∶0.25(v/v/v/v)的分离体系,对五种药物具有良好的分离效果。确定实验条件后利用TLC分离技术对样品溶液分别进行初步分离,在薄层板上不同比移值的斑点原位处滴加金胶进行SERS检测,对样品溶液在斑点原位处的SERS光谱进行采集、比较,确定。研究结果表明,五种沙坦类违禁添加成分可通过TLC明确分离,且其SERS光谱特征峰一致、重复性良好,根据各自的特征峰可快速定性分析,检出限在0.1~1 mg·kg^(-1)之间。研究建立的TLC-SERS方法简单、快速,能够为保健食品中违禁添加成分的现场初步快速筛查提供一定参考。Due to the current unhealthy diet structure and lifestyle habits,as well as the aging population and other factors,the incidence of chronic diseases such as hypertension is gradually increasing,and people gradually favor antihypertensive health food.However,in order to improve the efficacy of healthy food,there are unscrupulous businessmen in the market who illegally add antihypertensive drugs,especially sartans antihypertensive drugs,to healthy food.Based on the above phenomenon,this study established a Thin-Layer Chromatography(TLC)and Surface-enhanced Raman spectroscopy(SERS)method to investigate five possible prohibited ingredients of sartans(Olmesartan Medoxomil,Irbesartan,Losartan potassium,Telmisartan and Valsartan)in antihypertensive health food products.In this study,we investigated the optimal conditions for the SERS detection of five drugs,compared the effects of TLC spreaders with different ratios of different components on the separation of the five drugs.We successfully obtained the separation system of cyclohexane-ethyl acetate-methanol-glacial acetic acid=53∶35∶12∶0.25(v/v/v/v)after extensive formulation tests.After determining the exact conditions of this experiment,the preliminary separation of drug standard solution,mock positive sample solution and real sample solution was carried out by using TLC separation technique.After separation,gold gel was added dropwise at the spot in situ with different ratio shift values on the thin layer plate for SERS detection.The SERS spectra of drug standard solution as well as mock positive sample solution at the spot in situ were collected,compared and determined.The results showed that the five prohibited additive ingredients of sartans could be clearly separated by TLC,their SERS spectra were consistent and reproducible,and the qualitative analysis could be performed quickly according to their respective characteristic peaks,with detection limits between 0.1 and 1 mg·kg^(-1).The TLC-SERS method established in this study is simple and rapid.It can pro

关 键 词：降压类保健食品 沙坦类药物 薄层色谱层析-表面增强拉曼光谱联用技术 同步检测 

分 类 号：O657.37[理学—分析化学]