基于表面增强拉曼光谱的鸭肉中大环内酯类抗生素残留检测研究

发布时间：2018-07-22 10:24

【摘要】：农产品食品安全问题已在全世界范围内备受关注,鸭肉作为饲养量最大的水禽并且具有极高的营养价值,因而其抗生素滥用导致的食用安全问题更是人们关注的一个焦点,因此研究鸭肉中抗生素残留的快速检测方法具有十分重要的意义。表面增强拉曼光谱(SERS)法因其具有简便、快捷、灵敏度高等特点,已被广泛地应用在许多领域中。本文主要采用表面增强拉曼光谱法结合化学计量学法对鸭肉中的三种大环内酯类抗生素进行了快速检测研究,其主要研究内容及结果如下:(1)SERS定性定量快速检测鸭肉中螺旋霉素的残留。研究采用OTR202作为SERS活性基底,建立了螺旋霉素水溶液的快速检测定量分析模型,并以乙酸乙酯作为提取溶剂,确定了螺旋霉素的1622cm-1峰可以作为其在鸭肉提取液中残留检测的拉曼特征峰。然后进一步利用SERS结合自适应迭代重加权惩罚最小二乘法(air-PLS)快速检测鸭肉中的螺旋霉素残留,实验通过单因素分析法确定了最佳条件,并在此条件下建立了螺旋霉素浓度范围介于4.0~50.0mg/L之间的鸭肉提取液加标样本的标准曲线,并获得了良好的线性关系且线性回归方程为y=26.681x+1233.5,决定系数R2=0.9802,最低检测限为4mg/L,预测样本的平均回收率为73.38%~105.25%。(2)SERS定性定量快速检测鸭肉中替米考星的残留。研究采用OTR202作为SERS活性基底,建立了替米考星水溶液的快速检测定量分析模型,并以乙酸乙酯作为提取溶剂,经正己烷除脂、氮气吹除后得到鸭肉提取液,确定了替米考星的1584cm-1峰可以作为其在鸭肉中残留检测的拉曼特征峰。然后利用SERS结合air-PLS快速检测鸭肉中的替米考星残留,实验通过单因素分析法确定了最佳条件,并在此条件下建立了替米考星浓度范围介于2.0~50.0mg/L之间的鸭肉提取液加标样本的标准曲线,并获得了良好的线性关系且线性回归方程为y=0.0419x+0.8252,决定系数R2=0.9839,最低检测限为2mg/L,预测样本的平均回收率74.76%~102.59%。(3)SERS定性定量快速检测鸭肉中吉他霉素的残留。研究采用OTR202作为SERS活性基底,建立了吉他霉素水溶液的快速检测定量分析模型,并以乙酸乙酯作为提取溶剂,经正己烷除脂、氮气吹除后得到鸭肉提取液,确定了吉他霉素的1228和1268cm-1峰可以作为其在鸭肉中残留检测的拉曼特征峰。然后利用SERS结合air-PLS快速检测鸭肉中的吉他霉素残留,实验通过单因素分析法确定了最佳条件,并在此条件下建立了吉他霉素浓度范围介于4.0~40.0mg/L之间的鸭肉提取液加标样本的标准曲线,并获得了一定的线性关系且线性回归方程为y=0.0119x+0.9409,决定系数R2=0.9232,最低检测限为4mg/L,预测样本的平均回收率104.44%~108.35%。研究表明,采用SERS结合air-PLS建立鸭肉中螺旋霉素、替米考星和吉他霉素残留的快速检测研究方法是可行的。
[Abstract]:The problem of food safety of agricultural products has been paid close attention to all over the world. As the largest amount of waterfowl and high nutritional value, duck meat is the focus of attention because of the food safety caused by the abuse of antibiotics. Therefore, it is of great significance to study the rapid detection of antibiotic residues in duck meat. Surface enhanced Raman spectroscopy (SERS) has been widely used in many fields because of its simplicity, rapidity and high sensitivity. In this paper, surface enhanced Raman spectroscopy and chemometrics were used to study the rapid detection of three macrolides in duck meat. The main contents and results were as follows: (1) SERS was used to determine the residue of spiramycin in duck meat. Using OTR202 as the active substrate of SERS, a rapid quantitative analysis model of spiramycin aqueous solution was established, and ethyl acetate was used as the extraction solvent. The 1622cm-1 peak of spiramycin can be used as the Raman characteristic peak for detection of spiramycin residues in duck meat extract. Then SERS combined with adaptive iterative heavy weight penalty least square (air-PLS) method was used to detect spiramycin residues in duck meat quickly. The best conditions were determined by single factor analysis. Under these conditions, the standard curve of the duck meat extract added with standard sample was established, in which the concentration of spiramycin ranged from 4.0 to 50 mg / L, and the concentration of spiramycin was in the range of 5.0 mg / L. A good linear relationship was obtained. The linear regression equation was YY 26.681x 1233.5, the determination coefficient R20.902, the lowest detection limit 4 mg / L, and the average recovery rate of predicted samples was 73.38 and 105.25.The (2) SERS was used to determine the residues of telmicosin in duck meat qualitatively and quantitatively. Using OTR202 as the active substrate of SERS, a rapid quantitative analysis model of temicoxin in aqueous solution was established, and ethyl acetate was used as the extraction solvent, and the duck meat extract was obtained after n-hexane degreasing and nitrogen blowing. The 1584cm-1 peak of telmicosin can be used as the Raman characteristic peak of its residual detection in duck meat. Then SERS and air-PLS were used to detect the tenmicosin residues in duck meat. The best conditions were determined by single factor analysis. Under these conditions, the standard curve of the duck meat extract added with standard samples with the concentration range of 2.0 ~ 50.0 mg / L of telmicoxacin was established. A good linear relationship was obtained, and the linear regression equation was: yttria 0.0419x 0.8252, the determination coefficient R2N 0.9839, the lowest detection limit being 2mg / L, the average recovery of predicted samples was 74.76102.59. (3) SERS was used to determine the residue of guitar mycin in duck meat. Using OTR202 as the active substrate of SERS, a rapid quantitative analysis model of guitar mycin aqueous solution was established. Ethyl acetate was used as the extraction solvent, and the duck meat extract was obtained after n-hexane degreasing and nitrogen blowing. The peaks of 1228 and 1268cm-1 of Guitamycin can be used as the Raman characteristic peaks of the residue detection in duck meat. Then SERS and air-PLS were used to detect the guitar mycin residues in duck meat. The best conditions were determined by single factor analysis. Under these conditions, the standard curve of the duck meat extract with standard sample was established, in which the concentration of guitar mycin ranged from 4.0 to 40.0 mg / L. A certain linear relationship was obtained, and the linear regression equation was Y = 0.0119x 0.9409, the determination coefficient was R220.9232, the lowest detection limit was 4 mg / L, and the average recovery rate of the predicted sample was 104.440.108.35. The results showed that it was feasible to establish a rapid method for the detection of spiramycin, telmicosin and guitar mycin residues in duck meat by SERS and air-PLS.
【学位授予单位】：江西农业大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：S859.84

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