摘要
本研究比较了不同光引发剂在液相色谱-四极杆飞行时间质谱(LC-QTOF MS)和气相色谱-三重四极杆质谱(GC-MS/MS)中的响应灵敏度和稳定性,并依此建立了食品接触涂层中12种光引发剂迁移量的LC-QTOF MS测定方法和11种光引发剂迁移量的GC-MS/MS测定方法。对于LC-QTOF MS方法,采用酸化甲醇稀释样品后上机测试。采用Hypersil GOLD AQ色谱柱,以0.1%甲酸水-甲醇为流动相进行梯度洗脱,电喷雾离子源正离子(ESI+),多反应监测-高分辨(MRM HR)模式监测。方法检出限为0.002 5~0.01 mg/kg,回收率为60.9%~124%,相对标准偏差(RSD)为0.9%~11.6%。对于GC-MS/MS方法,采用正己烷萃取样品,萃取液上机测试。采用CD-5色谱柱,MRM模式监测。方法检出限为0.000 4~0.002 mg/kg,回收率为77.0%~128%,RSD为0.4%~8.1%。使用这2种方法检测13批次食品接触涂层样品的迁移液,其中在5份迁移液中检出光引发剂TPO和2,4-二乙基噻唑酮。本研究建立的方法前处理简单、灵敏度高,具有较好的准确性和精密度,适用于食品接触涂层制品中光引发剂的检测。
Photointiators have been commercially applied in ultra-violet photocuring ink,varnish,coating,lacquers since 1970s.The significant advantages of efficient,energy-saving and environmental-friendly make them more and more popular in automobile industry,package industry,etc.Photointiators can reach foodstuff by vapour or diffusion from the food contact layer of the package.Although UV ink is just printed in the outer surface of the package,the residue photointiators can transfer to the inner surface by“set-off”effect.Different photointiator has different chemical and physical properties,and shows different response by different testing instrument.In this study,two methods of liquid chromatography time-of-flight mass spectrometry(LC-QTOF MS)and gas chromatography triple quadrupole mass spectrometry(GC-MS/MS)were developed for determination of migration for 23 photoinitiators in food contact coating.The response of the photointiators by two methods was compared for method selection.For the LC-QTOF MS method,an Hypersil GOLD AQ C18 column was utilized and 0.1%formic acid water-methanol was used as mobile phase.QTOF MS was performed by electrospray ion source positive ion mode(ESI+)and mutiple reaction monitor high resolution(MRM HR)mode.Simple dilution with acidified methanol was used for migration solution pretreatment and internal standard method was used for quantification.The limits of detection are from 0.0025 to 0.01 mg/kg.Recoveries range from 60.9%to 124%,and the relative standard deviations(RSDs)are between 0.9%and 11.6%.For GC-MS/MS method,a CD-5 column was used,and the MS/MS was operated under MRM mode.Liquid-liquid extraction with n-hexane was used for migration solution pretreatment and internal standard method was also used for quantification.The limits of detection range from 0.0004 to 0.002 mg/kg.The recoveries range from 77.0%to 128%,with RSDs are between 0.4%and 8.1%.Migration solution of 13 batches of metal coating samples were tested,while 5 of them are positive of photoinitiaor TPO or 2,4-diethyl-9H-thioxanthen-9-one,while the maximum detection value of photoinitiaor TPO is 0.0502 mg/kg,the detection values of 2,4-diethyl-9H-thioxanthen-9-one are all less than 0.002 mg/kg.The two methods are easy,sensitive and accuracy,which can determine the migration of photointiators in food contact coating.
作者
熊小婷
饶璞
刘春生
陈意光
宋梓锋
林醇
李慧勇
黄晓钢
何国山
XIONG Xiao-ting;RAO Pu;LIU Chun-sheng;CHEN Yi-guang;SONG Zi-feng;LIN Chun;LI Hui-yong;HUANG Xiao-gang;HE Guo-shan(Collaborative Innovation Center for NQI-Quality Safety of Guangzhou,National Quality Inspection and Testing Center for Packaging Products(Guangzhou),Guangzhou Quality Supervision and Testing Institute,Guangzhou 511447,China;Guangzhou Institute for Food Inspection,Guangzhou 511410,China)
出处
《质谱学报》
EI
CAS
CSCD
北大核心
2024年第4期577-586,I0006,共11页
Journal of Chinese Mass Spectrometry Society
基金
广州市科技计划项目(2023B04J0407)
广东省市场监督局科技项目(2022CZ05)。
作者简介
通信作者:陈意光。
