A method for the simultaneous determination of 21 triazole fungicides in animal-origin foods was established by using UPLC–MS/MS. The dilution solvent, extraction solvent, and QuEChERS purification adsorbent composition, were optimized. The response value of the target compound was the highest and the chromatographic peak shape was optimal under the following conditions: water-acetonitrile as the mobile phase, acetonitrile to extract the target compound, C18 (100 mg) as the adsorbent, and water-acetonitrile as the diluent. Our method was validated under electrospray ionization (ESI) + conditions with six animal-origin foods. The 21 triazole fungicides showed good linear relationships (0.1–20 μg∙L−1, R2 > 0.99). The limits of detection and quantitation ranged from 0.1 to 0.3 μg∙kg−1 and 0.3 to 0.9 μg∙kg−1, respectively. The average recoveries ranged from 72.0% to 114.8% with RSDs < 9.9%. Therefore, our method was suitable for the determination of pesticide residues in commercially available animal-origin samples.
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