Simultaneous determination of acetylacetone and acetone in the reaction mixture for producing acetylacetone by high performance liquid chromatography

A method was developed for the simultaneous determination of acetylacetone and acetone in the reaction mixture for producing acetylacetone from ketene-acetone process by using reversed-phase high performance liquid chromatography. An Agilent Eclipse XDB-C18 column (150 mm×4.6 mm,5 μm) was used for the separation at the column temperature of 30 ℃. Tetrahydrofuran-water (15:85,v/v),including 0.1 mol/L monosodium phosphate,was used as the mobile phase (pH 4.0-5.0) at a flow rate of 0.6 mL/min. The detection was performed at 270 nm by an ultraviolet absorbance detector. The quantitative analysis was performed using an external standard calibration curve. Under the optimized conditions,the linear ranges for acetylacetone and acetone were 0.01-50.00 mg/L and 0.01-30.00 mg/L,respectively,and the correlation coefficients were both above 0.9999. The contents of acetylacetone and acetone were determined by this method. The repeatabilities of the analytical results were excellent and the relative standard deviations were less than 1.0%. The spiked recoveries of acetylacetone and acetone were 99.00%-101.50%. Compared with the ultraviolet spectrophotometric analysis of acetylacetone,the relative error was 1.48%. This method provides the basis for the determination of acetylacetone produced by acetone,as well as the similar mixed system. Simultaneously,it is simple,accurate and efficient for determining ketone compounds.