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.
关键词
糕点 /
白酒 /
糖精钠 /
表面增强拉曼光谱 /
快速检测
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Key words
pastry /
liquor /
saccharin sodium /
surface-enhanced Raman spectroscopy /
rapid detection
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参考文献
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脚注
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基金
广西食品药品监督管理局科学研究项目(桂食药科2017-8(直属))资助;食品安全地方标准制定(修订)项目(桂地标食2016005号)资助
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