The detection of pesticide residued in fruit is an important concern for consumers. Surface enhanced Raman spectroscopy (SERS) coupled with gold colloid was applied to analyze two kinds of pesticides (phosmet, chlorpyrifos) which were mainly used on the navel orange. The concentration of the phosmet samples of range from 3 to 33 mg/L and chlorpyrifos samples of range from 4 to 34 mg/L. Using Partial least squares (PLS) regression and the different preprocessing method for the spectral data analyses, and different pretreatment methods such as the Savitzky-Golay were compared. The optimal model of phosmet pesticide and chlorpyrifos pesticide were set up. The prediction correlation coefficient (R) and the root mean square error of prediction (RMSEP) of phosmet pesticide were 0.924 and 4.293 mg/L; The R and RMSEP of chlorpyrifos pesticide were 0.715 and 6.646 mg/L. It indicated that SERS technology is a effective method in the field of pesticide residue detection in fruit.