基于凝胶渗透色谱-气相色谱串联质谱法的食品包装印刷油墨中光引发剂的测定

Simultaneous Determination of 8 Photoinitiators in the Printing Inks Used in Food Plastic Packaging Materials with GPC-GC-MS/MS Method

本实验建立了同时测定食品包装印刷油墨中二苯甲酮(BP)、4-甲基二苯甲酮(MBP)、2-苯甲酰苯甲酸甲酯(OMBB)、4-二甲氨基苯甲酸乙酯(EDAB)、2-异丙基硫杂蒽酮(ITX)、4-二甲氨基苯甲酸-2-乙基己酯(EHA)、2,4-二乙基硫杂蒽酮(DETX)和4-氯二苯甲酮(CBP)等8种光引发剂(PIs)含量的凝胶渗透色谱(GPC)-气相色谱串联质谱(GC-MS/MS)方法。样品用环己烷-乙酸乙酯混合溶剂超声提取,提取溶液经GPC净化分离和富集以后,以50%苯基-50%甲基聚硅氧烷为固定相(Rtx-17MS),采用多反应监测(SRM)方式对上述8种光引发剂进行了定性和定量分析。8种光引发剂在0.2~100.0μg/L范围内的线性关系良好,线性相关系数大于0.9979;在3种浓度的添加水平下,回收率范围为80%~105%,相对标准偏差为2%~10%;方法的定量限为0.01~0.05mg/Kg。实验结果表明,采用该方法,样品前处理过程较简单,灵敏度高,准确度和精密度好,适用于食品料包装印刷油墨中8种光引发剂的检测要求。

A novel analytical method based on Gel permeation chromatography(GPC)-gas chromatography tandem mass spectrometry(GC-MS/MS) techniques was developed for the determination of eight photoinitiators(PIs) including benzophenone(BP),4-methylbenzophenone(MBP),Methyl o-Benzoylbenzoate(OMBB),Ethyl 4-dimethylaminobenzoate(EDAB),2-Isopropylthioxanthone(rrX),2-ethylhexyl-4-dimethylaminobenzoate(EHA),Diethylthioxanthenone(DETX) and 4-Chlorobenzophenone(CBP),in the printing inks used in food packaging.The packaging printing ink samples were firstly extracted by ultrasound-assisted extraction method using cyclohexane-ethyl acetate as the extraction solvents,and then purified and enriched by GPC.Qualitative and quantitative analysis were carried out for the analytes under the select reaction moniring(SRM) mode after the chromatographic separation on a 50% Phenyl-50% methylpolysiloxane(Rtx-17MS) Capillary chromatographic column.The linear plots ranged from 0.1 to 100 μg/L with correlation coefficients larger than 0.9979.By adding 3 different concentration of a standard mixture of PIs into the extracts of the blank packaging materials,the recoveries obtained were in the range of 80%~ 105%,with the relative standard deviations between 2% and 10%.The Umits of detection for the method were 0.01 ~0.05mg/kg.The results indicated that the newly-developed method is simple,fast,sensitive,accurate and suitable for the determination of 8 PIs in food packaging printing ink.