LC-MS/MS Determination of Migration of 18 Photoinitiators in Food Contact Paper Based Materials with Printing UV-Ink
摘 要
选取4%(体积分数,下同)乙酸溶液、50%(体积分数,下同)乙醇溶液、95%乙醇溶液和橄榄油作为食品模拟物,模拟了食品接触材料在与不同类型食物接触下的迁移行为。采用液相色谱-串联质谱法测定纸质食品接触材料印刷紫外固化油墨中18种光引发剂的迁移量。迁移试验得到的水基食品模拟液,经过滤后直接进样测定;油基食品模拟液需要经乙腈提取后进行测定。以C18色谱柱为分离柱,以不同体积比的0.1%(体积分数)甲酸溶液和0.1%(体积分数)甲酸乙腈溶液的混合液作为流动相进行梯度洗脱,质谱分析采用多反应监测模式对18种光引发剂的定量离子和定性离子进行监测。18种光引发剂的质量浓度均在3.0~37.5 μg·L-1内或质量分数均在0.010~0.125 mg·kg-1内与其对应的峰面积呈线性关系,在4%乙酸溶液、50%乙醇溶液、95%乙醇溶液及橄榄油食品模拟物中的测定下限(10S/N)分别为0.03~2.97 μg·L-1,0.02~2.91 μg·L-1,0.03~2.88 μg·L-1和0.06~9.00 ng·g-1。以空白样品为基体进行加标回收试验,所得回收率为86.0%~114%,测定值的相对标准偏差(n=6)不大于9.4%。
Abstract
4% (φ, the same below) acetic acid solution, 50% (φ, the same below) alcohol solution, 95% alcohol solution and olive oil were used as food simulants to simulate migration behavior of food contact materials in contact with different types of food. LC-MS/MS was applied to the determination of migration of 18 photoinitiators in food contact paper based materials with printing UV-ink. The aqueous food simulant solution was just filtered through filter before injection, and the oil food simulant solution was extracted by acetonitrile before determination. The solution was separated on C18 chromatographic column using a gradient elution program with the mixture of 0.1% (φ) formic acid solution and 0.1% (φ) formic acid in acetonitrile solution mixed in different ratios as mobile phase. The quantitative and qualitative ions of 18 photoinitiators were monitored by MS with multiple reactions monitoring. Linear relationships between values of peak area and mass concentration or mass fraction of 18 photoinitiators were kept in the same range of 3.0-37.5 μg·L-1 or 0.010-0.125 mg·kg-1, with lower limits of determination (10S/N) of 0.03-2.97 μg·L-1 for 4% acetic acid solution, 0.02-2.91 μg·L-1 for 50% alcohol solution, 0.03-2.88 μg·L-1 for 95% alcohol solution and 0.06-9.00 ng·g-1 for olive oil, respectively. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 86.0%-114%, with RSDs (n=6) of determined values no more than 9.4%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202007001
所属栏目 试验与研究
基金项目 上海市质量监督检验技术研究院项目(KY-2018-7-QH);上海市日用消费品质量安全检测专业技术服务平台(14DZ2293000)
收稿日期 2020/1/18
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备注袁琳嫣,工程师,研究方向为食品相关产品质量与安全检测以及相关的风险评估,yuanly@sqi.org.cn
引用该论文: YUAN Linyan,HAN Chen,LI Jiejun. LC-MS/MS Determination of Migration of 18 Photoinitiators in Food Contact Paper Based Materials with Printing UV-Ink[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(7): 745~754
袁琳嫣,韩陈,李洁君. 液相色谱-串联质谱法测定纸质食品接触材料印刷紫外固化油墨中18种光引发剂的迁移量[J]. 理化检验-化学分册, 2020, 56(7): 745~754
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【3】徐莹.食品包装行业中UV油墨光引发剂的危害、法规要求及其替代[J].绿色包装, 2017(10):54-58.
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【5】韩伟,庞震,张媛媛,等.超高压液相色谱法测定食品接触材料印刷油墨中光引发剂[J].食品安全质量检测学报, 2013,4(4):1005-1009.
【6】SHEN D X, LIAN H Z, DING T, et al. Determination of low-level ink photoinitiator residues in packaged milk by solid-phase extraction and LC-ESI/MS/MS using triple-quadrupole mass analyzer[J]. Analytical and Bioanalytical Chemistry, 2009,395(7):2359-2370.
【7】张居舟,陶固帅,尚光志,等.超高效液相色谱-串联质谱法测定食品塑料包装材料中5种光引发剂及其迁移规律[J].理化检验-化学分册, 2017,53(11):1246-1251.
【8】刘艳,张强,顾华,等.气相色谱-质谱同时测定食品包装材料中9种光引发剂[J].分析科学学报, 2017,33(6):812-816.
【9】徐文泱,陈华.气-质联用法同时检测高脂食品中14种光引发剂[J].食品与机械, 2018,34(8):54-59.
【10】徐文泱,刘漾伦,刘宇,等.气相色谱-质谱法检测湘式挤压糕点中4种光引发剂[J].食品安全质量检测学报, 2017,8(10):3980-3986.
【11】李中皓,吴帅宾,刘珊珊,等.超高效合相色谱法快速检测纸质印刷包装材料中10种受限制光引发剂[J].分析化学, 2013,41(12):1817-1824.
【12】陶运来,田素润.凝胶渗透色谱-气相色谱-串联质谱法测定牛奶中的两种光引发剂[J].化学分析计量, 2018,27(5):11-15.
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