| Poultry is a kind of food with high nutritional value,and it is also one of the indispensable foods in daily life.In poultry farming,antibiotics are inevitably used in order to prevent and treat various diseases of poultry.However,some antibiotics are not easily degraded,and unreasonable use will cause them to remain in poultry,which threatens people’s health.To ensure the quality and safety of poultry products,some scholars at home and abroad have been exploring and researching rapid detection technologies for antibiotic residues.Traditional methods for detecting antibiotic residues require complex preprocessing,long time and high cost,making it difficult to achieve rapid detection of antibiotic residues in poultry.In this work,poultry(chicken,duck meat)was used as a carrier,sulfamethazine(SM2),ofloxacin(OFL),danofloxacin mesylate(DFM),sarafloxacin hydrochloride(SARH)and doxycycline hydrochloride(DCH)were used as research objects.Synchronous fluorescence technology coupled with chemometric methods were used to explore a rapid detection method for antibiotic residues in poultry.The main research work is as follows:(1)The rapid detection for SM2 and OFL residues in poultry was achieved through synchronous fluorescence technology coupled with chemometric methods.First of all,three-dimensional synchronous fluorescence spectra of SM2 standard solution,OFL standard solution,poultry extract without antibiotics and poultry extract containing SM2and OFL were analyzed,and the wavelength difference(Δλ)of SM2 and OFL were respectively determined as 150 nm and 210 nm,and the fluorescence excitation peaks of SM2 and OFL were respectively determined as 292.5 nm and 295 nm for the detection of SM2 and OFL residues in poultry.Subsequently,the effects of the addition amounts ofβ-mercaptoethanol solution and o-phthalaldehyde solution,as well as time,on the fluorescence intensities were investigated through the single factor test.The best detection conditions of SM2 and OFL residues in chicken were as follows:β-mercaptoethanol solution of 300μL,o-phthalaldehyde solution of 25μL and time of 44 min.Besides,the best detection conditions of SM2 and OFL residues in duck meat were as follows:β-mercaptoethanol solution of 400μL,o-phthalaldehyde solution of 25μL and time of 40 min.Finally,the prediction models of SM2 and OFL residues in chicken were established through the algorithms of the peak height and peak area,respectively.The experimental results showed that the prediction model based on the peak height algorithm has the better comprehensive evaluation by comparison of the prediction model based on the peak area algorithm.For the prediction model of SM2 residues based on the peak height algorithm,the linear equation was y=0.550 5x+18.884.The coefficient of determination for the training set(R_T~2)and prediction set(R_P~2)were 0.919 4 and 0.897 3,respectively.The root mean square error for the prediction set(RMSEP)was 6.060 5 mg/kg,and the recovery was in the range of 76.1～115.2%,and the relative standard deviation(RSD)was in the range of 2.7～7.0%.For the prediction model of OFL residues based on the peak height algorithm,the linear equation was y=7.783 8x+15.919.The R~2_Tand R~2_Pwere 0.973 8 and0.997 3,respectively.The RMSEP was 0.539 2 mg/kg.The recovery and RSD were in the range of 96.7～110.1%and 2.8～10.0%,respectively.Besides,the prediction models of SM2 and OFL residues in duck meat were established through the algorithms of the peak height and peak area,respectively.The experimental results show that the comprehensive evaluation of the prediction model based on the peak height algorithm better than the prediction model based on the peak area algorithm.For the prediction model of SM2 residues based on the peak height algorithm,the linear equation was y=0.501 7x+19.049.The R~2_Tand R~2_Pwere 0.844 7 and 0.815 6,respectively.The RMSEP was 7.950 9 mg/kg.The recovery and RSD were in the range of81.7～155.1%and 4.1～6.7%,respectively.For the prediction model of OFL residues based on the peak height algorithm,the linear equation was y=7.320 6x+10.705.The R~2_Tand R_P~2were 0.996 6 and 0.996 2,respectively.The RMSEP was 0.526 7 mg/kg.The recovery and RSD were in the range of 96.4～111.2%and 2.9～6.8%,respectively.(2)The rapid detection for DFM and OFL residues in poultry was achieved through synchronous fluorescence technology coupled with chemometric methods.First of all,the synchronous fluorescence spectra of DFM standard solution,OFL standard solution,poultry extract without antibiotics and poultry extract containing DFM and OFL were analyzed,and theΔλof DFM and OFL were respectively determined as 130 nm and 200nm,and the fluorescence excitation peaks of DFM and OFL were respectively determined as 288 nm and 325 nm for the detection of DFM and OFL in poultry,respectively.Subsequently,the effects of the concentrations of sodium hydroxide solution and the type of surfactant on the fluorescence intensities were investigated through the single factor test.The best detection conditions of DFM and OFL residues in chicken were as follows:the concentration of sodium hydroxide solution of 0.1 mol/L,and the concentration of SDS solution of 0.1 mol/L.The best detection conditions of DFM and OFL residues in duck meat were as follows:the concentration of sodium hydroxide solution of 0.1 mol/L,and the concentration of SDS solution of 0.1 mol/L.Finally,the prediction models of DFM and OFL residues in chicken were established through the algorithms of the linear regression,partial least squares regression(PLSR),and multiple linear regression(MLR),respectively.The experimental results showed that the comprehensive evaluation of the prediction model of DFM residues based on the PLSR algorithm was best among these algorithms.The R~2_Pand RMSEP were 0.978 3 and 1.934 2mg/kg,respectively.The ratio of prediction to deviation(RPD)was 5.876 5.The comprehensive evaluation of the prediction model of OFL residues based on the MLR algorithm was best among these algorithms.The R_P~2,RMSEP,and RPD were 0.895 0,3.859 8 mg/kg,and 2.509 1,respectively.Besides,the prediction models of DFM and OFL residues in duck meat were established through the algorithms of the linear regression,PLSR,and MLR,respectively.The experimental results showed that the comprehensive evaluation of the prediction model based on the linear regression algorithm was best among these algorithms.For the prediction model of DFM residues based on the linear regression algorithm,the R_P~2,RMSEP,and RPD were 0.968 2,1.619 2 mg/kg,and 4.711 7,respectively.For the prediction model of OFL residues based on the linear regression algorithm,the R_P~2,RMSEP,and RPD were 0.964 3,2.244 0 mg/kg,and 4.751 3,respectively.(3)The rapid detection for SARH and DCH residues in chicken was achieved through synchronous fluorescence technology coupled with chemometric methods.First of all,three-dimensional synchronous fluorescence spectra of SARH standard solution,DCH standard solution,chicken extract without antibiotics and chicken extract containing SARH and DCH were analyzed,and theΔλof both SARH and DCH were determined as 110 nm,and the fluorescence excitation peaks of SARH and DCH were respectively determined as320 nm and 381 nm for the detection of SARH and DCH residues in chicken.Subsequently,the effects of the concentrations of magnesium sulfate solution and SDS solution,as well as time,on the fluorescence intensities were investigated through the single factor test.The best detection conditions of SARH and DCH residues in chicken were as follows:the concentration of magnesium sulfate solution of 0.375 mol/L,the concentration of SDS solution of 0.30 mol/L and time of 12 min.Finally,the prediction models of SARH and DCH residues in chicken were established through the algorithms of the MLR,PLSR,and support vector regression(SVR),respectively.The experimental results showed that the comprehensive evaluation of the prediction model based on the PLSR algorithm was best among these algorithms.For the prediction model of SARH residues based on the PLSR algorithm,the R_P~2,RMSEP,and RPD were 0.846 5,0.344 1 mg/kg,and 2.588 2,respectively.For the prediction model of DCH prediction based on the PLSR algorithm,the R_P~2,RMSEP,and RPD were 0.914 1,5.890 9 mg/kg,and 3.243 5,respectively.In this thesis,a method for the rapid detection of SM2,OFL,DFM,SARH,and DCH residues in poultry was explored using synchronous fluorescence technology combined with chemometric methods.Based on this,the application of synchronous fluorescence technology can be further optimized and expanded for the detection of other antibiotic residues in poultry. |
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