食品包装纸和纸巾纸中邻苯二甲酸酯类增塑剂的测定

Determination of Phthalates in Food Packaging Paper and Tissue Paper

目的建立快速溶剂萃取一气相色谱质谱联用法测定纸张中邻苯二甲酸二异丁酯（DIBP）、邻苯二甲酸二丁酯（DBP）和邻苯二甲酸二（2-乙基己基）酯（DEHP）的含量。方法对本地超市采购的11种食品包装纸和20种纸巾纸中这3种增塑剂的含量进行了测定。纸样前处理条件，萃取剂为正己烷，萃取温度为100℃，静态萃取时间为5min，循环次数为2次。质谱采用全扫描模式（m／z范围为50～600）用于色谱条件优化，采用选择离子监测模式（SIM）进行定量，各物质定量离子均为149。结果所有纸样均含有增塑剂，22种同时含3种增塑剂。3种增塑剂总含量范围为7．8～1876．8mg／kg。个别餐巾纸和抽纸DEHP含量高于欧盟对塑料和塑料制品中DEHP的限量。汉堡纸中增塑剂含量最低。结论建立的检测方法快速有效，应＂-3关注市售食品包装纸和纸巾纸中增塑剂的含量。建议制定标准及法规，给出相关纸样增塑剂限量等。纸中还有一些其他未知化合物，其安全性有待进一步研究。

Objective To develop an accelerated solvent extraction coupled with gas chromatography-mass spectrometry （ASE/GC-MS） method for the determination of the concentrations of diisobutyl phthalate （ DIBP）, dibutyl phthalate （DBP） and di（2-ethylhexyl） phthalate （DEHP） in the paper samples. Methods The paper samples included 11 samples of food packaging paper and 20 samples of tissue paper sold in local supermarket. The samples were pretreated using the accelerated solvent extraction （ASE） method. They were extracted by hexane at 100 ~C with two cycles of static extraction for 5 min. Af- terwards they were analyzed using gas chromatography-mass spectrometry （GC-MS）. The chromatographic conditions were op- timized using full scan mode with mass-to-charge ratio range of 50 - 600. The quantification was obtained using peak area of the product ion in selected ion monitoring （SIM） mode. The mass to charge （m/z） ratio of quantification was 149 for each phthalate. Results All the samples contained phthalates. 22 samples contained three phthalates simultaneously. The concentra-tions of total phthalates ranged from 7.8 to 1876.8 mg/kg. The concentrations of DEHP were higher than the DEHP content limit in plastic material or plastic articles set by EU. The concentrations of these phthalates in Hamburger paper were relatively lower. Conclusion The analysis method was efficient and time-saving. Attention should be paid to the concentrations of these phthalates in food packaging paper and tissue paper products in the market. It is suggested that new standards or regulations a- bout the content limit of each phthalate in food packaging paper and tissue paper should be established. There were other un- known compounds in the paper samples. The safety evaluation of these compounds should be investigated.