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本文分析了聚乙二醇6000-硫酸铵双水相体系对维生素 B3的最佳萃取条件，并结合荧光法对其进行测定。且在最佳萃取条件下进行荧光扫描确定最佳激发/发射峰为λex /em＝319．0nm/392．0nm。聚乙二醇6000-硫酸铵双水相体系对维生素B3的一次性萃取率在91％～93％之间，线性范围8．0×10-6～2．0×10-4g/L ，检出限为1．3×10-7g/L。该方法萃取率高、线性范围宽、检出限低，可维生素B3的分析测定。“,”This paper studies the different aqueous two -phase system of the extraction of vitamin B3 best conditions ,and on the method combined with fluorescence method .Mainly discussed the acidity ,extraction solvent type and dosage ,extraction time and influence faciors of extraction ratio ,and in the best extraction conditions with the fluorescent to determine the optimal scanning stimulate/emission peak .Adopt the Aqueous Two Phase Extraction Based On PEG -(NH4)2SO4 to extract VB3 ,then determine the fluorescence of organic part by λex/λem=319 .0/392 .0nm .Results :The results suggest that the extraction efficiencies of vitaminB3 between the PEG6000 -salt system was91% ~93% in one-step extraction .The extraction method gave linear dynamic ranges of 8 .0 × 10 -6~2 .0 × 10 -4g/L with detection limits of 1 .3 × 10 -7g/L .Conclusion :This method has dramatic advantages such as high extraction efficiency ,long linearity ,little detection limits etc ,ap-ply to the determination of vitamin B3