Fenton-荧光法快速测定食用油中PAEs总量的研究

A rapid approach of Fenton coupled with fluorescence spectrometry for the quantitative determination of total phthalate esters in edible oils

建立了一种Fenton氧化结合荧光法快速测定食用油中邻苯二甲酸酯(PAEs)的新方法。食用油样品中的PAEs经乙腈萃取浓缩、碱性条件下水解后,利用Fenton反应生成荧光性能较强的羟基邻苯二甲酸类物质进行间接荧光定量测定。对影响衍生化效率的水解条件及Fenton反应进行了优化。结果表明:优化条件下,该方法具有较高的灵敏度,较好的线性关系(R^2=0.999 2)及重复性(相对标准偏差0.35%~5.46%),检出限和定量限分别为0.05、0.15 nmol/mL,回收率在84.52%~100.13%之间。适合于食用油批量样品的PAEs总量安全初筛过程中的高通量测定。

A rapid approach of Fenton oxidation coupled with fluorescence spectrometry for the quantitative determination of total phthalate esters （PAEs） in edible oils was established. PAEs in edible oils were extracted by acetonitrile and hydrolyzed in aqueous alkaline solutions. Hydroxyphthalic acids with significant fluorescence properties were produced by the Fenton reaction and analyzed by fluorescence spectrometry. The experimental parameters relating to the efficiency of the derivative reaction such as hydrolysis conditions and Fenton reaction were optimized. The results showed that under the optimal conditions, the method had the items of high sensitivity, good linearity （R^2 = 0. 999 2 ） , and repeatability （RSD was in the range of 0.35% -5.46% ）. The limits of detection and quantity were 0.05 nmol/mL and 0.15 nmol/mL respectively, and the recoveries were in the range of 84.52% - 100. 13%. The approach was suitable for the high throughput determination in preliminary security screening of total PAEs in batch edible oil samples.