Fan Yingying, Liu Shuhui, Xie Qilong
College of Science, Northwest A&F University, No. 3 Taicheng Road, Yangling, Shaanxi 712100, China.
College of Science, Northwest A&F University, No. 3 Taicheng Road, Yangling, Shaanxi 712100, China; State Key Laboratory of Crop Stress Biology in Arid Areas, Yangling, China.
Talanta. 2014 Feb;119:291-8. doi: 10.1016/j.talanta.2013.11.023. Epub 2013 Nov 15.
A very simple, fast and environmentally friendly sample extraction method was proposed for the analysis of phthalate esters (PAEs, di-isobutyl phthalate (DIBP), dibutylphthalate (DBP), butylbenzylphthalate (BBP) and bis(2-ethylhexyl)phthalate (DEHP)) in alcoholic beverages by using conventional ionic liquid dispersive liquid-liquid microextraction. The samples were extracted by 160 μL 1-octyl-3-methylimidazolium hexafluorophosphate in the presence of appropriate amount of ethanol and 10% (w/v) sodium chloride solution; the enriched analytes in sedimented phases were analyzed by high performance liquid chromatography-diode array detector (HPLC-DAD). Under the optimum conditions, a satisfactory linearity (in the range of 0.02-1 μg mL(-1) for white spirits and 0.01-0.5 μg mL(-1) for red wines with the correlation coefficients (r) varying from 0.9983 to 1), acceptable recovery rates (88.5-103.5% for white spirits and 91.6-104.6% for red wines), good repeatability (RSD ≤ 8.0%) and low detection limits (3.1-4.2 ng mL(-1) for white spirits and 1.5-2.2 ng mL(-1) for red wines) were obtained. The developed method was successfully applied for the determination of the four PAEs in 30 white spirits and 11 red wines collected locally, and the DBP content in 63% (19:30) white spirits exceeded the specific migration limit of 0.3 mg kg(-1) established by international regulation.
提出了一种非常简单、快速且环保的样品萃取方法，用于分析酒精饮料中的邻苯二甲酸酯（PAEs，邻苯二甲酸二异丁酯（DIBP）、邻苯二甲酸二丁酯（DBP）、邻苯二甲酸丁苄酯（BBP）和邻苯二甲酸二（2-乙基己基）酯（DEHP）），该方法采用常规离子液体分散液液微萃取。在适量乙醇和10%（w/v）氯化钠溶液存在下，用160 μL 1-辛基-3-甲基咪唑六氟磷酸盐萃取样品；通过高效液相色谱-二极管阵列检测器（HPLC-DAD）分析沉淀相中富集的分析物。在最佳条件下，获得了令人满意的线性关系（白酒中为0.02 - 1 μg mL⁻¹，红酒中为0.01 - 0.5 μg mL⁻¹，相关系数（r）在0.9983至1之间）、可接受的回收率（白酒为88.5 - 103.5%，红酒为91.6 - 104.6%）、良好的重复性（RSD≤8.0%）和低检测限（白酒为3.1 - 4.2 ng mL⁻¹，红酒为1.5 - 2.2 ng mL⁻¹）。所建立的方法成功应用于本地收集的30种白酒和11种红酒中四种PAEs的测定，63%（19:30）的白酒中DBP含量超过了国际法规规定的0.3 mg kg⁻¹的特定迁移限量。
