A novel method for determining pp'-DDT, op'-DDT, pp'-DDE, and pp'-DDD contamination in animal fats (beef tallow, lard, and chicken fat) without using toxic organic solvents for sample preparation, followed by HPLC, has been developed. The sample is prepared by matrix solid-phase dispersion (MSPD) extraction with Toyobo-KF (R), an activated carbon fiber, as a new MSPD sorbent. The average recoveries (spiking levels: 0.2, 0.5, and 1.0 mu g g(-1)) ranged from 58 to 93%, with relative standard deviations of < 7%. The limits of quantitation were 0.18 mu g(-1).