This study establishes a method for rapid detection of clonidine and cyproheptadine in foods of animal origin. In order to obtain the best detection method, capillary zone electrophoresis (CZE), large volume sample stacking (LVSS), and sweeping-micellar electrokinetic capillary chromatography (sweeping-MEKC) were used respectively. The limits of detection (LODs) of clonidine and cyproheptadine by LVSS-CZE were 0.028 μg mL⁻¹ and 0.034 μg mL⁻¹, and those by sweeping-MEKC were 0.023 μg mL⁻¹ and 0.031 μg mL⁻¹, respectively. Compared with the CZE method, the two online pre-concentration technologies have greatly improved the detection sensitivity and achieved good enrichment results. However, compared with the sweeping-MEKC system, the LVSS system consumed a longer time and was greatly affected by the actual sample matrix. The sweeping-MEKC method was proved to be suitable for real sample analysis. Under the best sweeping-MEKC conditions, clonidine and cyproheptadine could be well separated within 8 min and good linear relationships in the range of 0.1–1.0 μg mL⁻¹ (r2 > 0.99) were obtained. This method was successfully applied to the determination of clonidine and cyproheptadine in animal-derived foods with the recoveries of 82.3%–90.1% and the relative standard deviations (RSDs) less than 3.11%. The sweeping-MEKC method is simple to operate and has great potential in the rapid detection of clonidine and cyproheptadine in animal-derived foods.
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