高效液相色谱法同时测定乙酰丙酮反应液中的乙酰丙酮和丙酮

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

建立了一种同时检测乙烯酮-丙酮法制乙酰丙酮反应液中乙酰丙酮和丙酮的高效液相色谱法(HPLC)。采用Agilent Eclipse XDB-C18色谱柱,以四氢呋喃-水(15∶85,v/v)溶液为流动相(用0.1mol/L磷酸二氢钠缓冲盐调节pH为4.0～5.0),流速0.6mL/min,紫外检测波长270nm,采用外标法定量。在优化的条件下,乙酰丙酮和丙酮的线性范围分别为0.01～50.00mg/L和0.01～30.00mg/L,相关系数均为0.9999以上。使用HPLC测定乙酰丙酮和丙酮的含量,其相对标准偏差均小于1.0%,结果表明方法的重复性好;反应液中添加乙酰丙酮和丙酮的加标回收率均为99.00%～101.50%。与应用紫外分光光度法测定乙酰丙酮的结果相比,平均相对误差为1.48%。所建立的方法为用丙酮生产乙酰丙酮等类似混合体系中乙酰丙酮的定量分析提供了依据,同时为酮类化合物的测定提供了准确、便捷的方法。

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.