An effective sample preparation procedure using an accelerated solvent extraction (ASE) procedure, followed by cleaning with melamine molecularly imprinted polymers solid-phase extraction (MISPE) was developed. A novel and highly sensitive ASE–MISPE–ultra-performance liquid chromatography (UPLC) method was developed for effective separation and simultaneous determination of dicyandiamide (DCD), cyromazine (CYR), and melamine (MEL) in complex animal tissue foods. Under optimized conditions, good linearity was achieved with a correlation coefficient (r) of 0.9999 in the range of at least two orders of magnitude. The limit of quantification of the method was 1.7 μg/kg, 5.0 μg/kg, and 3.2 μg/kg for DCD, MEL, and CYR, which was three orders of magnitude smaller than the maximum residue limits (MRLs). The intra- and inter-day precisions (in terms of the relative standard deviation, RSD) of the three analytes were in the range of 1.7–3.1% and 3.1–6.3%, respectively. The average recoveries of analytes from blank chicken, beef, mutton, pork, and pig liver samples spiked with the three levels varied from 91.2% to 107% with RSD of 1.7–8.3% for DCD, 89.0–104% with RSD of 2.1–6.1% for CYR, and 94.8–105% with RSD of 1.1–6.6% for MEL. The proposed method has the characteristics of speed, sensitivity, and accuracy, and can be used for the routine determination of DCD, CYR, and MEL at the μg/kg level in complex animal tissue foods. © 2016

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