A method was developed for the determination of paraquat (PQ) and diquat (DQ) in high moisture food crops. Samples were digested with 6M HCl, and the herbicides were isolated from the digest using pH-controlled silica solid phase extraction. The analytes were then determined by ion-pairing liquid chromatography with a silica analytical column, sodium chloride as the ion-pairing reagent, and acetonitrile as the organic modifier. A diode array UV absorbance detector was used to simultaneously quantify PQ and DQ at their respective maximum absorbance wavelengths, 257 and 310 nm. Average recoveries of PQ and DQ standards from 4 different crops fortified at 0.01-0.50 ppm levels ranged from 79.3 to 104.8%.