光谱学与光谱分析, 2015, 35 (4): 919, 网络出版: 2015-04-20  

表面增强拉曼光谱检测鸡蛋蛋清内三聚氰胺的定量方法研究

Quantitative Approach to Melamine Detection in Egg White with Surface-Enhanced Raman Spectroscopy
作者单位
1 华中农业大学工学院, 湖北 武汉 430070
2 国家蛋品加工技术研发分中心,华中农业大学, 湖北 武汉 430070
3 华中农业大学食品科学技术学院, 湖北 武汉 430070
4 欧普图斯(苏州)光学纳米科技有限公司, 江苏 苏州 215000
摘要
三聚氰胺对人体有害,鸡蛋内三聚氰胺定量检测非常有必要.以鸡蛋蛋清为研究对象,应用表面增强拉曼光谱技术结合化学计量学方法对蛋清内三聚氰胺进行了定量检测.首先采用人工饲养蛋鸡的方法获取含有三聚氰胺的样品鸡蛋.然后使用便携式拉曼光谱检测仪(Opto Trace RamTracer-200)和拉曼增强试剂测定蛋清的表面增强拉曼光谱,同时利用气相色谱质谱技术测定相应蛋清中三聚氰胺的含量.利用Raman Analyzer对拉曼光谱基线进行校正.应用相关系数法从表面增强拉曼光谱中选取320个光谱变量作为输入变量,建立偏最小二乘定量校正模型;并应用谱峰分解法建立谱峰分解定量校正模型.两种模型建立过程中均选定90个样本做为模型校正集,44个样本做为模型验证集,两种模型都有较好的预测效果.偏最小二乘定量校正模型预测值与气相色谱质谱联用法(GC-MS)测定值的决定系数R2为0.856,预测均方根误差RMSEP为1.547;谱峰分解定量校正模型R2为0.947,RMSEP为0.893.实验结果表明,该方法能有效定量检测鸡蛋内三聚氰胺,检测一个样本仅需15 min,为蛋品的三聚氰胺检测提供了一种新途径.
Abstract
Due to the harmfulness of melamine to human,the quantitative detection of melamine in egg is very necessary.In the present study,the surface enhanced Raman spectra technology combined with chemometric analysis method was used to conduct melamine quantitative detection in egg white.Firstly,the melamine egg sample could be got by the method of artificial feeding hens usingdifferent feeding formulation.Then the surface enhanced Raman spectra of egg white was determined using portable Raman spectroscopy (Opto Trace RamTracer-200) and Raman enhancement reagents,and the melamine content within the white eggs was measured with gas chromatography mass spectrometry technology.The software of Raman Analyzer was used for baseline correction of Raman spectra.The correlation coefficient method was used to choose 320 spectral variables from the surface enhanced Raman spectroscopy as input variables to establish partial least squares quantitative calibration model .And the peaks-decomposition method was used to establish peaks-decomposition quantitative calibration model.Both models selected 90 and 44 samples respectively as calibration sets and validation sets during model establishment,and both models achieved good prediction effect.The determination coefficient between predicted values of partial least squares quantitative calibration model and measured values of gas chromatography mass spectrometry was 0.856,and root mean square error of prediction was 1.547.The determination coefficient was 0.947 and RMSEP was 0.893 for the peaks-decomposition quantitative calibration model.This study demonstrated that the method can effectively quantitatively detect melamine in eggs.Testing a sample only takes 15 minutes,which can provide a new way for the melamine egg detection.

王巧华, 刘亚丽, 马美湖, 汪泓. 表面增强拉曼光谱检测鸡蛋蛋清内三聚氰胺的定量方法研究[J]. 光谱学与光谱分析, 2015, 35(4): 919. WANG Qiao-hua, LIU Ya-li, MA Mei-hu, WANG Hong. Quantitative Approach to Melamine Detection in Egg White with Surface-Enhanced Raman Spectroscopy[J]. Spectroscopy and Spectral Analysis, 2015, 35(4): 919.

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