Liu Pengyan, Huang Enjie, Chen Yanjie
College of Chemistry & Environmental Science, Hebei University, Baoding 071002, China.
Se Pu. 2012 Dec;30(12):1235-40. doi: 10.3724/sp.j.1123.2012.09001.
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 microm 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 microg/L. The linearity ranged from 0.03 to 1.0 microg/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 microg/dm2; 4-MBP was detected in ten samples, and the migration amounts of 4-MBP were from 0.006 to 0.019 microg/dm2; CPK was detected in three samples, and its amounts were 0.005, 0.005, 0.007 microg/dm2; 2,2-DMPA was detected as 0.009 microg/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.
从包装材料迁移到水溶性食品中的光引发剂(PI)的量通常非常小。使用目前的方法几乎检测不到。因此,本文描述了一种检测PI迁移的新有效方法。在该方法中,迁移实验在水性食品模拟物中进行。使用65微米聚二甲基硅氧烷/二乙烯基苯(PDMS-DVB)涂层纤维通过固相微萃取(SPME)从溶液中提取食品接触材料中使用的印刷油墨中的PI后,采用气相色谱-质谱联用仪(GC-MS)在选择离子监测模式(SIM)下测定其迁移量。通过SPME/GC-MS测定的PI有二苯甲酮(BP)、1-羟基环己基苯基酮(CPK)、4-二甲基氨基苯甲酸乙酯(EDMAB)、4-甲基二苯甲酮(4-MBP)、2,2-二甲氧基-2-苯基苯乙酮(2,2-DMPA)、2-苯甲酰基苯甲酸甲酯(OMBB)和2-乙基己基-4-二甲基氨基苯甲酸酯(EHDAB)。检测限(S/N = 3)在0.0012至0.0069微克/升之间。线性范围为0.03至1.0微克/升(r2 > 0.9909)。回收率在70.8%至112.0%范围内(n = 3),相对标准偏差不超过14.0%。使用该开发方法对20个样品进行了测试,分析结果表明,所有样品中均检测到BP,BP的迁移量为0.002至0.074微克/平方分米;10个样品中检测到4-MBP,4-MBP的迁移量为0.006至0.019微克/平方分米;3个样品中检测到CPK,其含量分别为0.005、0.005、0.007微克/平方分米;1个样品中检测到2,2-DMPA为0.009微克/平方分米。实际样品的测定表明该方法可行。该方法灵敏、简便且无需有机溶剂。可为食品包装表面印刷油墨中PI的迁移测定提供参考。