A new method for detecting carbaryl residues in duck meat is proposed using three- dimensional fluorescence spectroscopy and partialleastsquares regression (PLSR),according to the carbaryl derivatives with strong fluorescent properties. The two- dimensional contour spectrograms of samples are analyzed, the results indicate that the characteristic peaks of carbaryl and duck meat are separated obviously, which located at 300/365 nm and 320/460 nm in carbaryl-duck systemrespectively. Prediction model of carbaryl contents in the duck meat is established using PLSR, the coefficient of determination (R2) and the root mean squared prediction error (Prms) are 0.9883 and 3.103, respectively. The results show that the method which combining three- dimensional fluorescence spectroscopy with PLSR could be used to measure thecarbaryl residue in duck meat,it has the advantages of rapid and accuracy determination, and an effective means is provided for detection of pesticide residue in duck meat.