沉淀分离-气相色谱法快速测定PET包装材料中6种邻苯二甲酸酯

GC Determination of Six Phthalates in PET Packing Materials with Separation by Precipitation

为减少样品处理时间、快速测定聚对苯二甲酸乙二醇酯(PET)包装材料中邻苯二甲酸酯类塑化剂的含量,建立了沉淀分离-气相色谱法测定PET中6种邻苯二甲酸酯的方法。选用六氟异丙醇溶解PET试样,加对二甲苯沉淀分离聚合物基质,可有效提取目标物邻苯二甲酸酯,同时能消除基体干扰。提取液通过GC-FID法检测,6种邻苯二甲酸酯含量在0.50~100.0 mg/L范围内具有良好的线性响应关系。方法的定量限为5~13 mg/kg。在中、高含量水平下方法的相对标准偏差为2.2%~4.7%,在低含量水平下方法的相对标准偏差小于8%,不同含量水平下的加标回收率均在90.5%~103.5%之间。对于实际样品的测定,可以获得与现行国标法一致的结果。方法简便迅速,样品处理时间不足20 min,色谱测定时间约15 min。

In order to reduce sample treatment time and determine phthalate in polyethylene terephthalate （PET） packing materials rapidly, gas chromatography （GC） determination of six phthalates in PET packing materials with separation by precipitation was applied. PET specimen was dissolved with hexafluoroisopropanol, and the polymer was separated by precipitation with p-xylene, which could extract target objects phthalate and eliminate matrix interference effectively. GC-FID method was applied to detect extracting solution. Good linear response relations of six phthalates within concentration range of 0. 50 - 100. 0 mg/L. The detection limit was 5 - 13 mg/kg with concentrations, and the RSD under low concentration RSD of 2.2% ~ 4. 7% under medium and high was less than 8%. The recovery under different concentration levels was between 90. 5% - 103.5%. This method can obtain consistent results with the current GB method aiming at the determination of practical samples. More importantly, this method is simple and fast with sample handing time less than 20 rain and chromatozraDhic detection time about 15 min.