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The methodology for the identification and determination of 492 different toxicants from a single sample in food and feed by high-resolution quadrupole time-of-flight MS in combination with HPLC has been presented. The sample preparation is easy. The analytes are pesticides of different classes, including mycotoxins, veterinary drugs, and synthetic dyes. A scheme for the identification and determination of toxicants using the standard addition method has been given. The RSDs of the analytical results presented are ≤0.15, with a 40-60 min sample screening time and a 2-3 h for the determination of the detected toxicants.