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

摘要

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26 min内有效分离,且在0.01～5.00 mg/L范围内线性关系良好(R2＞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0.001～0.021 mg/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6.3%～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: 1) 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.