Abstract: A rapid high performance liquid chromatography (HPLC) method for simultaneous determination of sodium 5-nitroguaiacolate(SD1),sodium 4-nitrophenoxide dihydrate (SD2) and sodium 2-nitrophenoxide(SD3) in compound sodium nitrophenolate technical material(TC) was established. The optimum chromatographic conditions have been set up after examing the mobile phase and the detector wavelength.The determination was carried out on a Eclipse XDB C18 column (250 mm×4.6 mm,5 μm) with mobile phase V(methanol):V(water)=60:40, detection wavelength 335 nm,column temperature 30℃ and flow rate 1.0 mL/min. Complete separation of the above three comounds was achieved in 7.0 min under the optimized conditions.The developed method was fully validated.The peak purity factor of sodium 5-nitroguaiacolate,sodium 4-nitrophenoxide dihydrate and sodium 2-nitrophenoxide were all above 999 and the linear ranges were 0.6-286.7 mg/L,0.5-518.5 mg/L and 0.5-272.0 mg/L, respectively,with their correlation coefficients greater than 0.999.The limit of quantitation (LOQ) were 0.6,0.5 and 0.5 mg/L.The contents of the three compositions were 15.8%,50.0% and 33.0%,with their relative standard deviations 1.7%,1.0% and 1.3%,respectively.The optimized and validated method is efficient,accurate and easy to use,which provides theory basis and reliable method for determination and quality control of compound sodium nitrophenolate TC.