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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1 031cm-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,1 031cm-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=293.31 X+435.42,决定系数R2为0.933 7。真实值与预测值之间的R2为0.964 3,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%。
In order to achieve a rapid detection of streptomycin sulfate residues in water, a surface enhanced Raman spectroscopy (SERS) method for the determination of STR in aqueous solution was developed. The Au nanocapsules made of HAucl4 were reduced by trisodium citrate as the surface-enhanced substrate by induction heating. The absorption spectra of Au nanocrystals, the SERS of STR aqueous solution and the assignments of Raman peaks were analyzed. Finally, the Raman peak at 1 031cm-1 was taken as the characteristic peak to establish the calibration curve of STR aqueous solution and verify the accuracy and accuracy of the calibration curve . The experimental results showed that there was a good linear relationship between the Raman peak intensity at 1 031 cm-1 and the concentration of STR aqueous solution when the concentration of STR in water was 2.0-20.0 mg / L, the linear equation was Y = 293.31 X + 435.42 , The coefficient of determination R2 is 0.933 7. The R2 between the true value and the predicted value was 0.964 3, the root mean square error (RMSEP) was 1.3043 mg / L, the recovery was 92.1-133.0%, and the relative standard deviation (RSD, n = 5) was 0.88-2.41%.