Naturally contaminated corn samples of different origin were extracted using two conventional techniques (blending and shaking) and three alternative approaches (ultrasonic extraction, accelerated solvent extraction, and microwave-assisted extraction). Use of the same extraction mixture for all trials enabled the efficiency of the various extraction techniques to be compared. Extracts were filtered and directly analyzed by LC–ESI–MS, without further clean-up. The yield from the alternative extraction techniques showed efficiency to be higher than for conventional techniques. In particular, microwave-assisted extraction was slightly superior to other techniques.