相转移催化水解-超分子溶剂萃取法测定食用油中邻苯二甲酸酯总量

Determination of Total Phthalates in Edible Oil by Phase Transfer Catalyst Assisted Hydrolysis and Supramolecular Solvent Extraction

建立了食用油中邻苯二甲酸酯总量的快速测定方法。在四丁基氯化铵的催化作用下,油样中的邻苯二甲酸酯水解为邻苯二甲酸,进一步利用辛醇、四氢呋喃和水形成的超分子溶剂萃取,采用高效液相色谱-串联质谱法（HPLC-MS/MS）定量分析。本方法的水解时间为10 min,目标物的线性范围为50~2000μg/L（r〉0.999）,检出限（LOD）为5.1μg/kg,定量限（LOQ）为18μg/kg,3个水平加标回收率为84.6%~104.5%,日内及日间精密度分别为2.6%和3.7%。选择12种实际油样进行测定,邻苯二甲酸酯总含量范围为0.30~1.09 mg/kg。

A new method for the rapid determination of total phthalates （PAEs） in edible oils was developed. The PAEs in edible oils all were hydrolyzed to phthalic acid with tetrabutylammonium chloride （TBAC） as catalyst. Then phthalic acid was extracted by the supramolecular solvent （ SUPRAS） made up of octanol, tetrahydrofuran and aqueous solution, and detected by high performance liquid chromatography-tandem mass spectrometry （HPLC-MS / MS）. As a result, hydrolysis time was 10 min. The linear range of phthalic acid was 0. 05- 2. 0 mg / L with a good correlation coefficients （ r 〉 0. 999）. The limits of detection （ LOD） and quantification （LOQ） were 5. 41 and 18. 05 μg / kg, respectively. The recoveries of target analyte at three spiked levels were in the range of 84. 6% - 104. 5% . The repeatability, expressed as relative standard deviation （RSD）, was 2. 6% for intra-day and 3. 7% for inter-day. The total PAEs content of 12 edible oils was found in the range of 0. 30-1. 09 mg / kg.