GC-MS/MS法测定间接包装材料中18种光引发剂向改性聚苯醚模拟物的迁移量

Determination of Migration of 18 Photoinitiators in Indirect Packaging Materials to Simulator of Modified Polyphenylene Oxide by GC-MS/MS

为了研究间接包装材料中光引发剂（PIs）的迁移规律，建立了采用改性聚苯醚（MPPO）作为模拟物的迁移实验方法，并通过气相色谱-串联质谱（GC-MS／MS）联用技术测定了18种PIs的特定迁移量。间接包装材料中迁移出的PIs被MPPO吸附后，用乙腈萃取，萃取液用正己烷-乙酸乙酯（3：7，体积比）进行溶剂置换后，经有机滤膜过滤和DB-5MS弹性毛细管色谱柱分离后，采用串联质谱法分析，内标法定量。结果表明：①18种PIs在26min内有效分离，且在0．01~5．00mg／L范围内线性关系良好（R^2〉0．997）。加标回收率在86．4％～123．8％之间，相对标准偏差（RSD）〈8．3％，检出限（LOD）为0．001-0．021mg／kg。②迁移量在0．02～30．00μg／g时，该测试方法相对重复性标准偏差在613％～21．4％之间，相对再现性标准偏差在13．5％～22．3％之间。③实际样品PIs的迁移率与其分子量和沸点显著负相关。④真空镀铝内衬纸可以有效地阻隔PIs的迁移。

In order to study the migration of photoinitiators （PIs） in the indirect packaging materials, a GC-MS/MS method was developed to determine the specified migration of 18 PIs, modified polyphenylene oxide （MPPO） was used as a simulator. PIs adsorbed by MPPO was extracted with acetonitrile, the extract then was solvent-displaced by n-hexane-ethyl acetate （v/v 3：7）, filtered with organic filter membrane, separated on DB-5MS capillary column, analyzed by MS/MS and quantified by inner standard. The results showed that： l） All of the 18 PIs were well separated in 26 min and had good linear relationship （R2〉 0.997） within 0.01-5.00 mg/L. The recoveries of 18 PIs ranged from 86.4% to 123.8% with relative standard deviation less than 8.8% and the limits of detection （LODs） from 0.001 to 0.021 mg/kg. 2） Within the migration range of 0.02-30.00 μg/g, the relative standard deviation of repeatability and reproducibility ranged between 6.3%-21.4% and 13.5%-22.3%, respectively. 3） The migration rates of PIs in real samples significantly negatively correlated to their molecular weights and boiling points. 4） Vacuum aluminized inner liner could effectively barrier PIs migration.