食品包装材料中7种光引发剂向水性模拟液中的迁移测定

为了考察食品包装材料中光引发剂向食品中迁移的情况,以水性模拟液作为迁移溶剂,用65 μm聚二甲基硅氧烷/二乙烯基苯(PDMS-DVB)纤维头进行固相微萃取结合气相色谱-质谱(SPME/GC-MS)分析方法同时测定食品包装材料中7种光引发剂(PIs)的迁移量。方法的检出限为0.0012～0.0069 μg/L,线性范围为0.03～1.0 μg/L (r2＞0.9909),在3种浓度的添加水平下,加标回收率为70.8%～112.0%,相对标准偏差不大于14.0%。利用建立的方法对20个实际样品进行测定,发现所有样品中均检出二苯甲酮,其中10个样品中检出4-甲基二苯甲酮,3个样品中检出1-羟基环己基苯基甲酮,1个样品中检出安息香双甲醚。该方法的灵敏度高,样品前处理过程简单,无需使用有机溶剂,为食品接触材料表面印刷油墨中PIs向水性样品中的迁移测定提供了参考。

Determination of the migration of seven photoinitiators in food packaging materials into aqueous solvent

The quantity of photoinitiators (PIs) migrated into hydrosoluble foods from packaging materials is usually very small. It is hardly detectable by using the current methods. For this reason, the article describes a new effective method for detecting the migration of PIs. In this method, the migration experiment was done in aqueous food simulation. After the PIs in printing inks used in food contact materials were extracted from the solution via solid-phase microextraction (SPME) using 65 μm polydimethylsiloxane/divinylbenzene (PDMS-DVB)-coated fiber, their migration amounts were determined by gas chromatography-mass spectrometry (GC-MS) in the selected ion monitoring mode (SIM). The PIs determined by SPME/GC-MS were benzophenone (BP), 1-hydroxycyclohexyl-phenylketone (CPK), ethyl-4-dimethyl-aminobenzoate (EDMAB), 4-methylbenzophenone (4-MBP), 2,2-dimethoxy-2-phenylacetophenone (2,2-DMPA), methyl 2-benzoylbenzoate (OMBB) and 2-ethylhexyl-4-dimethyl-aminobenzoate (EHDAB). The limits of detection (S/N=3) were between 0.0012 and 0.0069 μg/L. The linearity ranged from 0.03 to 1.0 μg/L (r2＞0.9909). The recoveries were in the range from 70.8% to 112.0% (n=3) with the relative standard deviations no more than 14.0%. Twenty samples were tested by using this developed method. The analytical results showed that BP was detected in all samples, and the migration amounts of BP were from 0.002 to 0.074 μg/dm2; 4-MBP was detected in ten samples, and the migration amounts of 4-MBP were from 0.006 to 0.019 μg/dm2; CPK was detected in three samples, and its amounts were 0.005, 0.005, 0.007 μg/dm2; 2,2-DMPA was detected as 0.009 μg/dm2 in one sample. The determination of real samples showed this method is feasible. The method is sensitive, simple and free from organic solvents. It could make reference to migrating determination of PIs in printing inks on food packaging surface.