Study On Detection Of Macrolide Antibiotics Residue In Duck Meat Based On SERS

Food safety problem of agricultural products has received much attention in the whole world, as the largest amount of feeding waterfowl, duck also has a high nutritional value. The security issues caused by the abuse of antibiotics has become the focus of attention, so it is important to study the method for rapid detection of antibiotic residue in duck meat. Surface enhanced Raman spectroscopy(SERS) method has a widely application in many fields for the advantage of simple, rapid and high sensitivity. In this paper, the SERS method combined with chemometrics method was used for a rapid detection study on three kinds of macrolide antibiotic residue in duck meat, and the main contents and results are as follows:(1) Rapid detection study on quantitative and qualitative analysis of spiramycin residue in duck meat by using SERS method. In this research, OTR202 was used as SERS active substrate to establish the quantitative analysis model of rapid detection for spiramycin solution. The ethyl acetate was used as extraction solvent, and the Raman characteristic peak 1622cm-1 was considered as the detection basis for spiramycin residue in duck meat extract. Then the SERS method combined with the adaptive iterative re-weighted penalized least squares(air-PLS) method was further used for rapid detection of spiramycin residue in duck meat. The optimum experimental conditions were determined by single factor experiment. Under these conditions, the duck meat extract spiked samples of spiramycin concentrations range of 4.0~50.0mg/L were analyzed, and the standard curve was established and a good linear relationship was obtained. The linear regression equation was y=26.681x+1233.5, and the coefficient of determination(R2) was 0.9802. The detection limit was 4mg/L, and the average recoveries rate was 73.38%~105.25%.(2) Rapid detection study on quantitative and qualitative analysis of tilmicosin residue in duck meat by using SERS method. In this research, OTR202 was used as SERS active substrate to establish the quantitative analysis model of rapid detection for tilmicosin solution. The ethyl acetate was used as extraction solvent, and the duck meat extract was obtained after hexane degreasing and nitrogen blow-off, then the Raman characteristic peak 1584cm-1 was considered as the detection basis for tilmicosin residue in duck meat. Then the SERS method combined with air-PLS method was further used for rapid detection of tilmicosin residue in duck meat. The optimum experimental conditions were determined by single factor experiment. Under these conditions, the duck meat extract spiked samples of tilmicosin concentrations range of 2.0~50.0mg/L were analyzed, and the standard curve was established and a good linear relationship was obtained. The linear regression equation was y=0.0419x+0.8252, and the R2 was 0.9839. The detection limit was 2mg/L, and the average recoveries rate was 74.76%~102.59%.(3) Rapid detection study on quantitative and qualitative analysis of kitasamycin residue in duck meat by using SERS method. In this research, OTR202 was used as SERS active substrate to establish the quantitative analysis model of rapid detection for kitasamycin solution. The ethyl acetate was used as extraction solvent, and the duck meat extract was obtained after hexane degreasing and nitrogen blow-off, then the Raman characteristic peak 1228 and 1268cm-1 were considered as the detection basis for kitasamycin residue in duck meat. Then the SERS method combined with air-PLS method was further used for rapid detection of kitasamycin residue in duck meat. The optimum experimental conditions were determined by single factor experiment. Under these conditions, the duck meat extract spiked samples of kitasamycin concentrations range of 4.0~40.0mg/L were analyzed, and the standard curve was established and a linear relationship was obtained. The linear regression equation was y=0.0119x+0.9409, and the R2 was 0.9232. The detection limit was 4mg/L, and the average recoveries rate was 104.44%~108.35%.The research showed that it was feasible to establish the rapid detection of spiramycin, tilmicosin and kitasamycin residue in duck meat by using SERS combined with air-PLS.