为实现快速检测水中硫酸链霉素(STR)的残留,探索建立一种STR水溶液的表面增强拉曼光谱(SERS,surface enhanced Raman spectroscopy)检测方法。应用电磁炉加热以柠檬酸三钠还原氯金酸(HAucl4)制成的Au胶纳米颗粒作为表面增强基底,先后分析了Au胶纳米颗粒的吸收光谱、STR水溶液的SERS以及拉曼峰归属;然后确定了最佳的光谱仪功率、Au胶纳米颗粒的加入量和吸附时间;最后以1031cm-1处拉曼峰作为特征峰建立STR水溶液的标定曲线,并对标定曲线的准确度和精确度进行验证。实验结果表明,当水中STR质量浓度范围为2.0~20.0mg/L时,1031cm-1处的拉曼峰强度与STR水溶液的质量浓度有良好的线性关系,线性方程为Y=293.31X+435.42,决定系数R0为0.9337。真实值与预测值之间的R0为0.9643,均方根误差(RMSEP)为1.3043mg/L,回收率为92.1~133.0%,相对标准偏差(RSD,n=5)为0.88~2.41%。
A new method using surface enhanced Rarnan spectroscopy (SERS) was established for the rapid determination of streptomycin residues in water. The Au nanoparticles, which were prepared via sodium citrate deoxidizing tetrachloroauratetrihydrate with electromagnetic heating,were used as SERS substrate. Firstly, the absorption spectra of the Au nanoparticles, the SERS spectra of streptomycin solu- tion and its vibrational assignment were analyzed. And then the spectrometer's power, the addition a- mount of Au nanoparticles and the adsorption time were determined, respectively. Finally, the 1031 era-1 was used as the characteristic peak to establish the standard curve of streptomycin solution, and the pre- cision and accuracy of the standard curve were verified. The results show that a good linearity is obtained between the peak intensity at 1031 cm-1 and streptomycin solution concentration (2. 0-20. 0 nag/L), the linear equation is Y= 293. 31X+435.42, and the determination coefficient is 0. 933 7. The determination coefficient of streptomycin solutions between the actual values and the predictive values is 0. 964 3, and the root mean square error (RMSEP) is 1. 304 3 mg/L. Recovery rate of streptomycin residues in water is 92.1 %- 133. 0%, and the relative standard deviation is between 0. 88 % and 2.41 % (n= 5). It is feasible that the Au nanoparticles are used as the surface substrate and the Rarnan spectroscopy is used for the rapid determination of streptomycin residues in water.