The method of near-infrared, attenuated total reflectance infrared and Raman spectroscopy was used for the rapid determination of the content of deltamethrin in agrochemicals. The quantitative models were established by PLS (partial least squares) method and optimized. The independent validation sets were used to evaluate the model accuracy. The determination coefficient R2 and RMSECV of the near-infrared model and mid-infrared model were 0.999 9, 0.022 and 0.999 6 and 0.056, respectively. The accuracy of both was similar. The determination coefficient R2 and RMSECV of Raman were 0.996 7 and 0.172, which exhibits the lower accuracy. The result indicated that near-infrared, mid-infrared and Raman spectroscopy can be applied to the rapid determination of the content of the active ingredients precisely, which has an important significance in the on-line determination, analysis on site in the enterprise and the rapid quantitative analysis of agrichemicals in the department of quality monitoring.