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目的采用纳米金胶和OTR103作为表面增强拉曼光谱(surface-enhanced Raman spectroscopy,SERS)的活性基底,实现鸭肉中土霉素残留量的快速检测。方法首先使用自适应迭代惩罚最小二乘法(adaptive iterative re-weighted penalized least squares,air-PLS)扣除SERS测定过程中的荧光等背景信号,确定鸭肉中土霉素检测的特征峰。然后应用单变量分析法对纳米金胶、待测样品、OTR103的加入量和吸附时间进行优化,确定最佳实验条件。结果拉曼位移为1271 cm~(-1)处的特征峰可以作为鸭肉中土霉素残留检测的拉曼特征峰,纳米金胶、待测样品和OTR103的最适加入量分别为0.7 m L、70μL和100μL,最佳吸附时间为5 min。鸭肉中的土霉素浓度范围为0.2~22.0 mg/L时,土霉素浓度(X)与其在1271 cm~(-1)处的SERS特征峰强度(Y)之间有良好的线性关系,线性回归方程为Y=245.24X+647.29,决定系数(RC2)为0.9891,检测限为0.2 mg/L。预测集样本中土霉素含量的真实值与预测值之间的决定系数(RP2)为0.9941,均方根误差(RMSEP)为1.1341 mg/L,回收率为74%~102%。结论该方法可用于鸭肉中土霉素残留的快速检测。
OBJECTIVE To rapidly detect oxytetracycline residues in duck meat by using nano-Au and OTR103 as active substrates for surface-enhanced Raman spectroscopy (SERS). Methods Firstly, the background signal of fluorescence such as fluorescence was subtracted by adaptive iterative re-weighted penalized least squares (air-PLS) to determine the characteristic peak of oxytetracycline detection in duck meat. Then, unimodal analysis method was used to optimize the addition amount and adsorption time of nano gold gum, sample to be tested, OTR103, and determine the best experimental conditions. Results The characteristic peak at Raman shift of 1271 cm -1 could be used as the Raman peak of oxytetracycline residues in duck meat. The optimal addition amounts of nano gold gum, test sample and OTR103 were 0.7 m L, 70μL and 100μL, the best adsorption time is 5 min. There was a good linear relationship between the concentration of oxytetracycline (X) and the SERS peak intensity (Y) at 1271 cm -1 in duck meat with oxytetracycline concentration ranging from 0.2 to 22.0 mg / L , The linear regression equation was Y = 245.24X + 647.29, the determination coefficient (RC2) was 0.9891, and the detection limit was 0.2 mg / L. The determination coefficient (RP2) between the true value and the predicted value of the oxytetracycline content in the predictive set was 0.9941, the root mean square error (RMSEP) was 1.1341 mg / L and the recovery was 74% -102%. Conclusion The method can be used for the rapid detection of oxytetracycline residues in duck meat.