OBJECTIVE: To identify a new adulterated dye, and to establish simultaneous detection method for 9 orange-yellow dyes in Typhae Pollen. METHODS: TLC and LC-MS were used for the identification of the new adulterated dye; TLC and HPLC method were used for determining 9 orange-yellow dyes. The determination was performed on Welch AQ-C18 column with mobile phase consisting of acetonitrile-0.05 mol/L ammonium acetate solution (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelength were set at 432 nm (lemon yellow, metanil yellow, gold orange O, basic orangeⅡ) and 484 nm (sun-set yellow, acid orange Ⅰ, gold orangeⅡ, orange G, basic orange 21). The column temperature was 35 ℃.The sample size was 10 μL. RESULTS: TLC spots of auramine O, lemon yellow and new adulterated dye were clear and well separated without interference from negative control; new adulterated dye was identified as metanil yellow. TLC spots of lemon yellow, sunset yellow, orange G, acid orangeⅠ, gold orangeⅡ, auramine O, metanil yellow, basic orange 21 and basic orangeⅡwere clear and well separated without interference from negative control. The limits of detection were 0.30, 0.20, 0.33, 0.16, 0.19, 0.19, 0.31, 0.26, 0.30 mg/kg. CONCLUSIONS: The established method is able to detect adulterated dye and orange-yellow dye in Typhae Pollen rapidly and accurately.