光散射学报, 2019, 31 (1): 19, 网络出版: 2019-04-16
表面增强拉曼光谱快速检测糕点及白酒中糖精钠的研究
Rapid Detection of Saccharin Sodium in Pastry and Liquor by Surface-Enhanced Raman Spectroscopy
糕点 白酒 糖精钠 表面增强拉曼光谱 快速检测 pastry liquor saccharin sodium surface-enhanced Raman spectroscopy rapid detection
摘要
本研究建立了表面增强拉曼光谱快速检测糕点及白酒中糖精钠的方法。基于溶剂萃取法, 利用二氯甲烷对糕点及白酒中的糖精钠进行提取, 制备金溶胶后将其浓缩作为增强基底, 并优化增强基底的条件来获得最佳拉曼信号。结果表明, 在1.0 mol/L稀盐酸的酸性条件下用二氯甲烷提取糖精钠, 再用0.1 mol/L氢氧化钠溶液适当调节体系酸度后将糖精钠从二氯甲烷中反萃取出来, 可获得最高提取效率; 将1.0 mol/L稀硝酸作为凝聚剂使浓缩金溶胶与糖精钠分子紧密结合后检测, 可获得响应最强的SERS信号。糖精钠在糕点和白酒中的的最低检测浓度分别为0.5 mg/kg和0.5 mg/L, 回收率在75%~120%, RSD(n=5)在3.3%~8.6%, 该方法灵敏度高, 特异性强, 前处理方式简单, 实现了糕点及白酒中糖精钠的快速检测。
Abstract
A method for rapid determination of saccharin sodium in pastry and liquor was established by surface-enhanced Raman spectroscopy(SERS).Based on the solvent extraction method, dichloromethane was used to extract saccharin sodium from pastry and liquor.The concentrated gold colloid was prepared to use as Raman substrate, and the conditions of substrate was optimized.The results showed that saccharin sodium was extracted with dichloromethane under the acidic condition of 1 mol/L HCl, and saccharin sodium was back-extracted with 0.1 mol/L NaOH solution through adjusting the acidity of the system.When 1.0 mol/L HNO3 was used as coagulant to combine the concentrated gold colloid with saccharin sodium, the SERS signal with the strongest response could be obtained.The LOD of saccharin sodium in pastry and liquor were 0.5 mg/kg and 0.5mg/L respectively.And the recovery rate was between 75%~120% and RSD(n=5) was between 3.3~8.6%.So this method can be used for the rapid determination of saccharin sodium in pastry and liquor with the merit of high sensitivity, strong specificity and simple pretreatment method.
覃文霞, 余婉松, 郑娟梅, 袁光蔚, 王海波, 刘珈伶. 表面增强拉曼光谱快速检测糕点及白酒中糖精钠的研究[J]. 光散射学报, 2019, 31(1): 19. QIN Wenxia, YU Wansong, ZHENG Juanmei, YUAN Guangwei, WANG Haibo, LIU Jialing. Rapid Detection of Saccharin Sodium in Pastry and Liquor by Surface-Enhanced Raman Spectroscopy[J]. The Journal of Light Scattering, 2019, 31(1): 19.