分子荧光结合多维校正测定小龙虾中氨基脲残留量

Determination of Semicarbazide Residues in Crayfish by Molecular Fluorescence Combined with Multi-way Calibration Method

近年来,食品中的抗生素残留是人们关心的食品安全问题之一。为测定小龙虾中氨基脲残留量(SEM),本文提出一种基于三维荧光结合化学计量学测定小龙虾中SEM残留量的方法。样本经过简单的前处理,使用2-羟基-1-萘甲醛(2-HN)与SEM进行衍生化反应,生成具有荧光性质的2-羟基萘醛呋喃西林代谢衍生物(SEM-HN)。采集样本的荧光光谱,获得三维荧光数据矩阵;扣除空白样,采用平行因子分析(PARAFAC)算法和交替三线性分解算法(ATLD)对三维荧光数据矩阵进行分析,两种算法均能得到较好的定量分析结果。为了评估两种算法的准确性,对品质因子:灵敏度(SEN)、选择性(SEL)、检出限(LOD)和预测均方根误差(RMSEP)进行计算,结果表明两种算法准确性较好。为进一步验证PARAFAC算法和ATLD算法的性能,采用椭圆置信区间(EJCR)检验,结果本试验中ATLD算法优于PARAFAC算法。结论:三维荧光结合ATLD算法可快速测定小龙虾中的SEM残留。

In recent years,the problem of antibiotic residues in food is one of the food safety problems that people are concerned about.To determine the residue of semicarbazide(SEM)in crayfish,this study provides a method for the determination of SEM residues in crayfish based on Excitation-emission matrix fluorescence combined with chemometrics.After simple pretreatment,the sample was derivatized with 2-hydroxy-1-naphthylaldehyde and SEM to produce 2-hydroxy-naphthylaldehyde nitrofuran metabolites derivative(SEM-HN)with fluorescence properties.The fluorescence spectrometer collects the fluorescence spectra of the sample to obtain the three-dimensional fluorescence data matrix.After the blank sample was deducted,the excitation-emission matrix fluorescence data matrix was analyzed using PARAFAC and ATLD in chemometrics.Both algorithms can get better quantitative analysis results.In order to evaluate the accuracy of the two algorithms,the quality factors were calculated:sensitivity(SEN),selectivity(SEL),detection limit(LOD)and predicted root mean square error(RMSEP).The results show that the accuracy of the two algorithms is good.In order to further verify the performance of PARAFAC and ATLD,EJCR test analysis is used.The results show that ATLD algorithm is better than PARAFAC algorithm.Excitation-emission matrix fluorescence combined with ATLD algorithm can quickly determine SEM residues in crayfish.