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A quantitive assay for the determination of Xylidine Ponceau 2R was established by high performance liquid chromatography (HPLC) with solid phase extraction. Xylidine Ponceau 2R was extracted by alcohol-ammonia, solid phase extraction was utilized to cleanup. The separation was performed in a XDB-C18 column, acetonitrile, 5mmol/L ammonium acetate and 0.06% triethylamine as mobile phase. A photo-diode array detector was used to detect the compositions at 504 nm. The linear range of the method was 0.1~15 mug/mL, the limit of detection was 0.02 mg/L, the relative standard deviation was 0.33-2.86% and the average recoveries were 90.66~93.89%. The method was accuracy, sensitivity and feasibility to analyze the residues of Xylidine Ponceau 2R in foodstuffs.