Simultaneous Determination of Residues of 10 Photoinitiators in Ultroviolet Curing Offset Ink for Eoo-Friendly Cigarette Labels by Gas Chromatography-Mass Spectrometry
摘 要
用油墨打样机模拟实际印刷过程,以油墨定量仪控制胶印紫外光固化油墨的用量,制成了具有一定厚度的油墨样品。在剪碎的样品中加入乙腈和氘代蒽内标溶液,超声40 min。上清液经体积比3:7的正己烷-乙酸乙酯混合溶液萃取后,用装有150 mg无水硫酸镁、50 mg C18和50 mg N-丙基乙二胺的净化管净化。离心,取上清液过0.45 μm滤膜,所得滤液以40:1的分流比进样,在DB-5MS石英毛细管色谱柱(30 m×0.25 mm,2.5 μm)上以程序升温条件分离其中10种光引发剂,并用质谱仪检测。结果显示:10种光引发剂在26 min内可实现有效分离,标准曲线的线性范围为0.4~10.0 mg·L-1,检出限(3s)为0.25~1.5 mg·m-2;以实际样品为基质,3个浓度水平下的加标回收率为89.5%~105%,测定值的相对标准偏差(n=6)不大于7.0%。采用此方法分析蓝、红、黄和黑色油墨印制的样品,在红、黄和黑色油墨印制的样品中检出了二苯甲酮,最高检出量为0.39 mg·m-2,未超过标准YQ 69-2015规定的限量(20 mg·m-2)。
Abstract
An ink-scraping instrument with amount of ultroviolet curing offset ink controlled by ink meter was adopted for simulation of actual printing process to prepare ink samples with definite thickness. The cut sample obtained was taken and extracted ultrasonically with addition of acetonitrile and internal standard solution of deuterated anthracene for 40 min. The supernatant was extracted with mixed solution of n-hexane-ethyl acetate with volume ratio of 3:7, and purified with a purification tube containing 150 mg anhydrous MgSO4, 50 mg C18 and 50 mg N-propyl ethylene diamine. After centrifugation, the supernatant was passed through 0.45 μm filtrating membrane. The obtained filtrate was injected with split ratio of 40:1, and 10 photoinitiators were separated on DB-5MS quartz capillary column (30 m×0.25 mm, 2.5 μm) under temperature-programmed conditions, and detected by mass spectrometer. As shown by results, 10 photoinitiators could be effectively separated within 26 min, and linear ranges of the standard curves of 10 photoinitiators were 0.4-10.0 mg·L-1, with detection limits (3s) in the range of 0.25-1.5 mg·m-2. Test for recovery by standard addition method using actual sample as matrix was made at 3 concentration levels and results of recovery of 10 photoinitiators ranged from 89.5% to 105%, with RSDs (n=6) of the determined values not more than 7.0% . The proposed method was used for analyzing the samples prepared with blue, red, yellow and black inks, and benzophenone was detected in the samples prepared with red, yellow and black inks, with maximum detection amount of 0.39 mg·m-2, which did not exceed the limit (20 mg·m-2) specified in standard of YQ 69-2015.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202202007
所属栏目 工作简报
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收稿日期 2020/11/11
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备注王玉,硕士,主要研究方向为印刷复制技术
引用该论文: WANG Yu,LI Ying,LI Haishan,WANG Jing. Simultaneous Determination of Residues of 10 Photoinitiators in Ultroviolet Curing Offset Ink for Eoo-Friendly Cigarette Labels by Gas Chromatography-Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2022, 58(2): 161~165
王玉,李莹,李海山,王静. 气相色谱-质谱法同时测定环保型烟标胶印紫外光固化油墨中10种光引发剂的残留量[J]. 理化检验-化学分册, 2022, 58(2): 161~165
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参考文献
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【9】李中皓,唐纲岭,王庆华,等.超高效液相色谱法测定卷烟包装纸中的二苯甲酮和4-甲基二苯甲酮[J].现代食品科技, 2011,27(10):1276-1280.
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【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】袁琳嫣,杨建平,赵镭.液相色谱-串联质谱法检测纸质食品接触材料印刷UV油墨中18种光引发剂的残留量[J].食品安全质量检测学报, 2020,11(4):1065-1071.
【13】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.
【14】赵镭,袁琳嫣,韩陈.气相色谱-质谱法测定食品包装行业用UV油墨中11种光引发剂的含量[J].食品安全质量检测学报, 2020,11(7):2162-2167.
【2】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.
【3】DI GIANNI A, BONGIOVANNI R, PRIOLA A, et al. UV-cured fluorinated coatings for plastics:Effect of the photoinitiator and of the substrate filler on adhesion[J]. International Journal of Adhesion and Adhesives, 2004,24(6):513-518.
【4】RHODES M C, BUCHER J R, PECKHAM J C, et al. Carcinogenesis studies of benzophenone in rats and mice[J]. Food and Chemical Toxicology, 2007,45(5):843-851.
【5】BARNES K, RICHARD S C, WATSON D. Chemical migration and food contact materials[M]. Oxford:CRC Press, 2007.
【6】韩伟,于艳军,李宁涛,等.气相色谱-质谱法测定食品接触材料表面印刷油墨中的光引发剂[J].色谱, 2011,29(5):417-421.
【7】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.
【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】李中皓,唐纲岭,王庆华,等.超高效液相色谱法测定卷烟包装纸中的二苯甲酮和4-甲基二苯甲酮[J].现代食品科技, 2011,27(10):1276-1280.
【10】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.
【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】袁琳嫣,杨建平,赵镭.液相色谱-串联质谱法检测纸质食品接触材料印刷UV油墨中18种光引发剂的残留量[J].食品安全质量检测学报, 2020,11(4):1065-1071.
【13】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.
【14】赵镭,袁琳嫣,韩陈.气相色谱-质谱法测定食品包装行业用UV油墨中11种光引发剂的含量[J].食品安全质量检测学报, 2020,11(7):2162-2167.
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