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食品研究与开发:2017,38(19):161-165
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SERS检测三聚氰胺的不确定度分析
刘晓莹1,郑大威1,张萍1,*,师炜2,林太凤1,王惠琴1,曹智1
(1.北京工业大学生命科学与生物工程学院,北京100124;2.北京市密云区食品药品监督管理局,北京 101500)
Uncertainty Analysis of SERS Determination of Melamine
LIU Xiao-ying1,ZHENG Da-wei1,ZHANG Ping1,*,SHI Wei2,LIN Tai-feng1,WANG Hui-qin1,CAO Zhi1
(1.College of Life Science and Bioengineering,Beijing University of Technology,Beijing 100124,China;2.Food and Drug Administration of Beijing Miyun District,Beijing 101500,China)
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投稿时间:2017-01-22    
中文摘要: 不确定度是一类表征测试结果可靠性的重要参数,对于规范试验操作具有重要意义。表面增强拉曼光谱技术(surface enhanced Raman spectroscopy,SERS)作为一种用于物质定性和半定量分析的分子振动光谱,具有快速、简便和灵敏度高等特点,在食品安全与质量控制领域中广泛应用。利用SERS技术对三聚氰胺进行测定试验,并对该方法的不确定度进行分析。经辨识,确认715 cm-1处的峰为三聚氰胺的特征峰,该峰的峰强与三聚氰胺的浓度呈正相关。选取675 cm-1处的峰为内标峰,在0.1 μg/mL~5.0 μg/mL范围内,以I715/I675和浓度为参数进行线性回归分析。标准方程相关系数达到0.995 4,该方法的检出限为0.068 6 μg/mL。围绕标准工作曲线的建立,分析SERS测定三聚氰胺结果的不确定度来源并对其进行评定。通过不确定度分析,为确保测定结果的可比性与溯源性提供了参考价值。
Abstract:Uncertainty is a class of important parameters to represent the reliability of the measurement results.It has an important significance to standardize the experimental operation.Surface enhanced Raman spectroscopy(SERS)is a molecular vibrational spectroscopy for both qualitative and semi-quantitative detection of analytes.Recently,SERS had been widely used in the food safety and quality control areas owning to its several merits of fast detection,simple sample preparation,high sensitivity,etc.The quantitative detection of melamine had been established using SERS,and the uncertainty of SERS method had been analyzed meanwhile.Melamine showed the characteristic Raman peak at 715 cm-1steadily when mixed with Au nanoparticles.And the peak intensity of 715 cm-1had a positive relationship with the concentration of melamine.Taken 675 cm-1as the internal standard peak,there was a linear regression between I715/I675and the concentration of melamine in the range of 0.1 μg/mL-5.0 μg/mL.The correlation coefficient was 0.995 4,and the detection limit reached 0.068 6 μg/mL.The major uncertainty of SERS method was calculated and which mainly arise from the establishing of the standard curve by the least square method.Uncertainty analysis of SERS method would be benefit for the comparability and traceability of the measurement results.
文章编号:201719035     中图分类号:    文献标志码:A
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