Study On Detection Of Penicillin Residues Using SERS In Duck Meat

The problem of animal food safety has became more and more serious in recent years, and received the general concern of the world people, where one of the focuses of attention is the poultry food safety issues. As a kind of poultry food, duck meat has become indispensable good food in peoples’ life, and one of the main sources of duck safety problem is antibiotics residues. In duck-raising process, penicillin is often used as a class of antibiotics for the advantage of strong antibacterial effect, low toxin and lower price. Due to the abuse of penicillin in duck-raising process, the phenomenon of penicillin residues in duck is more and more serious. Therefore, it is very urgent to establish a method for the rapid detection of penicillin residues in duck meat. In recent years, surface enhanced Raman spectroscopy(SERS) method has been widely used as spectroscopy analysis technique with high sensitivity, quick analysis and no damage, which has been applied to the detection of antibiotics by many scholars. In this paper, the SERS method with Au nanoparticles was used to qualitatively analyze and quantitatively analyze the nafcillin, amoxicillin trihydrate and benzylpenicillin potassium residues in duck meat, and the rapid detection method of penicillin residues in duck meat were obtained. This study provided a basis for the application of SERS technology in poultry detection of penicillin residues, and the main research contents and results are as follows.(1) Research used ethyl acetate as the extraction solvent and Au nanoparticles A as SERS active substrate to establish a SERS method for the rapid detection of nafcillin and amoxicillin residues in duck meat.The different nano-sol on SERS effect of nafcillin and amoxicillin trihydrate in solutions was analyzed. The reductant addition(trisodium citrate) on SERS effect of nafcillin and amoxicillin trihydrate in solutions and different heating methods on SERS effect of nafcillin in solutions was discussed, respectively. Finally, the optimal SERS active substrate(Au nanoparticles A) was determined, and The UV-vis absorption spectra of the Au nanoparticles were characterized.Through the study on SERS of nafcillin in solutions, the Raman characteristic peaks using the characterization of nafcillin residues were determined, and their vibrational assignments were analyzed. The SERS of nafcillin in solutions and duck meat extract were comparing analysed, and the Raman characteristic peaks at 521, 948, 1059, 1145, 1240 and 1449cm-1 were used as Raman characteristic peak for the characterization of nafcillin residues in duck meat. The Raman intensities of nafcillin residues in duck meat extract at 521cm-1 and 1449cm-1 were used for the optimization of detection conditions. The peak intensity ratio of nafcillin residues in duck meat extract at 521cm-1 and 1449cm-1 was used to quantitatively analyze under the optimal conditions. The research found that there was a good linear relationship when the concentration range of nafcillin residues in duck meat extract was 0.2~10.0 mg/L, The linear equation was y=0.6215x+1.2491, and the determination coefficient(R2) was 0.9541. The detection limit was 0.2mg/L, and the average recoveries rate was 104~116%.Through the study on SERS of amoxicillin trihydrate in solutions, the Raman characteristic peaks using the characterization of amoxicillin trihydrate residues were determined, and their vibrational assignments were analyzed. The SERS of amoxicillin trihydrate in solutions and duck meat extract were comparing analysed, the Raman characteristic peaks at 553, 845, 948 and 1176cm-1 were used as Raman characteristic peak for the characterization of amoxicillin trihydrate residues in duck meat. The Raman intensities of amoxicillin trihydrate residues in duck meat extract at 845 and 1176cm-1 were used for the optimization of detection conditions. The peak intensity ratio of amoxicillin trihydrate residues in duck meat extract at 845cm-1 and 1028cm-1 was used to quantitatively analyze under the optimal conditions. The research found that there was a good linear relationship when the concentration range of amoxicillin trihydrate residues in duck meat extract was 0.2~10.0 mg/L, The linear equation was y=0.2017x+0.1582, and R2 was 0.9661. The detection limit was 0.2mg/L, and the average recoveries rate was 96~139%.(2) Research used acetonitrile as the extraction solvent and Au nanoparticles B as SERS active substrate to establish a SERS method for the rapid detection of benzylpenicillin potassium residues in duck meat.Through the study on SERS of benzylpenicillin potassium in solutions, the Raman characteristic peaks using the characterization of benzylpenicillin potassium residues were determined, and their vibrational assignments were analyzed. The different roughnesses of Au nanoparticles on SERS effect of benzylpenicillin potassium in solutions were discussed. The optimal SERS active substrate(Au nanoparticles B) was determined, and The UV-vis absorption spectra of Au nanoparticles and its mixture were characterized.The SERS of benzylpenicillin potassium in solutions and duck meat extract were comparing analysed, the Raman characteristic peaks at 993cm-1 and 1492cm-1 were used as Raman characteristic peaks for the characterization of benzylpenicillin potassium residues in duck meat. The Raman intensities of benzylpenicillin potassium residues in duck meat extract at 993 and 1492cm-1 were used for the optimization of detection conditions. The peak intensity of benzylpenicillin potassium residues in duck meat extract at 993cm-1 was used to quantitatively analyze under the optimal conditions. The research found that there was a good linear relationship when the concentration range of benzylpenicillin potassium residues in duck meat extract was 0.5~15.0 mg/L. The linear equation was y = 831.68 x + 1997.1, and R2 was 0.9441. The detection limit was 0.5mg/L, and the average recoveries rate was 90~121%.The research showed that it was feasible that SERS with Au nanoparticles was used for the rapid detection of nafcillin, amoxicillin trihydrate and benzylpenicillin potassium residues in duck meat,and this method could achieve the rapid detection of penicillin residues in duck meat.