摘要
目的 建立食品包装用印刷油墨中乙二醇醚类及酯类物质的气相色谱/质谱测定方法。方法 采用固相微萃取技术对油墨中的乙二醇醚进行富集, 对萃取方式、 萃取纤维、 萃取温度、 搅拌速率等参数进行优化。结果 涂层为65 μm的聚二甲基硅氧烷/二乙烯基苯萃取纤维的效率较高, 优化后的搅拌速率为250 r/min, 萃取温度为60 ℃, 萃取时间为15 min, 解吸温度为275 ℃, 解吸时间为3 min。结论 7种化合物在其质量浓度范围内呈良好的线性关系, 相关系数均大于0.99, 该方法的检出限为2.5~15.0 ng/L, 加标回收率为90.1%~99.9% , 相对标准偏差为5.2%~10.1%。该方法的样品前处理简便、 快速, 可用于食品包装用油墨中乙二醇醚及其酯类物质的检测。
Abstract
The aim of this work was to establish a GS/MS determination method for glycol ethers and their esters in printing inks used for food packaging. The glycol ethers in inks were enriched by solid-phase microextraction, and the parameters such as extraction mode, extracting fiber, extraction temperature and stirring speed were optimized. The polydimethylsiloxane/divinylbenzene extracting fiber with 65 μm coating showed the highest efficiency. The optimized stirring speed was 250 r/min, extraction temperature was 60 ℃ , extraction time was 15 min, desorption temperature was 275 ℃ , and desorption time was 3 min. All 7 compounds showed good linearity in their mass concentration ranges, with correlation coefficients of above 0.99. The detection limits for the components ranged from 2.5 ng/L to 15.0 ng/L, and the recoveries for spiked samples were between 90.1% and 99.9% with RSDs of 5. 2% to 10.1%. This method had simple and rapid sample pretreatment, and could be used for detection of glycol ethers and their esters in printing inks used for food packaging.
吕刚, 李晶, 张彬, 曹丽静.
油墨中乙二醇醚类物质检测[J]. 包装工程(技术栏目). 2015(7): 1-4
LYU Gang, LI Jing, ZHANG Bin, CAO Li-jing.
Determination of Glycol Ethers and Their Esters in Inks[J]. Packaging Engineering. 2015(7): 1-4
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基金
国家质检总局科技计划 (2013IK213)