整体柱承载形态对柯衣定SERS检测效果的影响

徐燕英 余慧 谢云飞等

摘要[目的]针对食品中屡禁不止的违禁添加色素柯衣定，拟建立一种以整体柱为活性增强基底、适合大批量样品快速筛查的表面增强拉曼散射（SERS）技术。[方法]在确定整体柱的合成后，以整体柱的柱状及其粉碎后的粉末为基底，优化金溶胶与样品的混合比例、体系pH、取样量和检测时间，分别建立柯衣定SERS检测方法。[结果]以整体柱的柱状及其粉碎后的粉末为基底分别建立柯衣定的SERS检测方法，其检测限分别为0.10和0.25 μg/mL；在10.0 μg/mL浓度下，柯衣定在整体柱柱状和粉状承载形态下获得的整体增强效果相近，1 138和1 171 cm-1处峰位移在柱状SERS检测中的信号强度明显优于粉状SERS检测结果，且柱状的SERS信号更稳定。[结论]建议采用整体柱的柱状形态进行SERS检测，更具实用价值，有望应用于大批量样品进行快速筛查。

关键词整体柱；表面增强拉曼（SERS）；柯衣定

中图分类号TS207文献标识码A文章编号0517-6611（2016）04-020-04

Effects of Bearing Forms of Monolithic Column on the SERS Detection of Chrysoidine

XU Yanying1，2， YU Hui2， XIE Yunfei2，3 YAO Weirong2* et al （1. Market Supervision Administration of Gusu District， Suzhou， Jiangsu 215100； 2. School of Food Science and Technology， Jiangnan University， Wuxi， Jiangsu 214122；3. Jiangsu Kangzhi Yuan Grain and oil Group Co.，LTD，Suqian，Jiangsu 223600）

Abstract[Objective] To establish a Surfaceenhanced Raman Spectroscopy （SERS） technology for rapid screening of mass samples， with monolithic column as the active substrate. [Method] After ensuring that the monolithic column was synthesized， the detection conditons were optimized based on different bearing forms of monolithic column， including the ratio of gold colloids to sample， pH of system， and Raman detection time. SERS detection method of chrysoidine was established. [Result] With the cylindricity and powder of monolithic column as the substrates， SERS detection limits were 0.10 and 0.25 μg/mL respectively. Under the 10.0 μg/mL concentration， their enhancing effects were close. Signal strengths of 1 138 and 1 171 cm-1 peak shifts in cylindricity SERS detection were significantly superior to those in powder SERS detection.And the cylindricity SERS signal was more stable. [Conclusion] Cylindricity of monolithic column should be used for SERS detection， which has greater practical value， and can be applied in the rapid screening of mass samples.

Key wordsMonolithic column； Surfaceenhanced Raman Spectroscopy； Chrysoidine

由于天然色素在食品加工過程中容易变色，工业染料柯衣定（别名：碱性橙II）价格低廉，颜色鲜艳，易溶于水，比其他人工合成色素，如日落黄、柠檬黄等更容易对食品上色且不易褪色，因此容易被一些不法商贩滥用于黄鱼、豆制品、腐竹、辣椒粉等食品中。目前柯衣定的检测方法主要有高效液相色谱法[1]、超高效液相色谱-串联质谱法[2]、液相色谱-串联质谱法[3]、反相高效液相色谱法[4]、薄层色谱扫描法[5]、比色法[6]等，均不适合对大批量样品进行快速筛查。

拉曼光谱（Raman spectroscopy）能够提供分子振动能和转动能方面的信息，每种物质在单色强光照射下均能产生特定的分子振动能和转动能变化，产生独一无二的拉曼光谱，因而能对物质进行指纹定性乃至定量鉴定。……