离子液体单滴微萃取-超高效液相色谱联用测定食品塑料包装材料中5种邻苯二甲酸酯的研究

Ionic liquid-based single-drop microextraction coupled with ultra-high performance liquid chromatography for determination of five phthalate esters in food plastic packaging materials

建立了一种基于离子液体单滴微萃取技术结合超高效液相色谱(IL-SDME-UPLC)对5种邻苯二甲酸酯类物质(PAEs)进行检测的方法,并成功应用于食品塑料包装材料中 PAEs 的分析。实验分别考察了离子液体种类、离子液体用量、萃取时间、萃取温度及盐效应对 PAEs 萃取效果的影响。结果表明,以30 uL 1-辛基-3-甲基咪唑六氟磷酸盐([C_8MIM][PF_6])为萃取剂,在25℃恒温水浴振荡5 min,不加入 NaCl 的条件下萃取效果最佳。在此优化条件下,结合 UPLC 测定了油桶及饮料瓶中的五种PAEs。结果显示,五种 PAEs 在2~100μg/mL 浓度范围内线性良好,相关系数R^2>0.999,方法的检出限为0.3~0.92μg/mL(S/N=3)。在10、20、30μg/mL 三个浓度水平下的加标回收率 DMP 为37.42%~43.50%;DBz P为65.04%~76.90%;DBP为67.22%~79.88%;DCHP为77.60%~89.82%;DOP为81.07%~87.62%,相对标准偏差(RSD)为0.01%~6.66%(n=3)。该方法绿色、简便、快捷、可操作性强,适用于食品塑料包装材料中邻苯二甲酸酯类的分析检测。

Ionic liquid single-drop microextraction coupled with ultra-high performance liquid chromatography （IL-SDME- UPLC ） was developed for extraction and determination of five phthalate esters （PAEs） from food plastic packaging materials. Several important influencing factors on IL-SDME extraction efficiency were investigated, such as the type of ionic liquid, amounts of extraction solvent, extraction time and temperature and salt solution concentration. The results indicated that the optimal experimental conditions were reached under 30 poL 1- oetyl-3- methylimidazolium hexafluorophosphates （[ CsMIM ] [ PF6 ] ）as extraction solvent without adding salt after oscillation 5 minutes at 25 ~C.The above-mentioned optimal method was successfully applied to the detection of the five PAEs in oilcan and beverage bottle.The results showed excellent linearity at 2-100 μg/mL concentration rang for the five PAEs.The coefficients of correlation were no less than 0.999 and the limits of detection ranged from 0.3 μg/mL to 0.92 μg/mL（ S/N = 3 ）.The recovery rates of five PAEs at three different spiked levels of 10,20,30 μg/mL were up to 37.42%-43.50% of DMP,65.04% -76.90% of DBzP,67.22%-79.88% of DBP, 77.60% - 89.82% of DCHP and 81.07% -87.62% of DOP with RSD in the range of 0.01% -6.66% （ n = 3 ） , respectively.The method was suitable to determine PAEs in food plastic packaging materials with environment-friendly characterization ,convince ,rapid and high operability.