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

Simultaneous Determination of Residues of 10 Photoinitiators in Ultroviolet Curing Offset Ink for Eoo-Friendly Cigarette Labels by Gas Chromatography-Mass Spectrometry

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 C_(18)和50 mg N-丙基乙二胺的净化管净化。离心,取上清液过0.45μm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,2.5μm)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))。

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 MgSO_(4),50 mg C_(18) and 50 mg N-propyl ethylene diamine.After centrifugation,the supernatant was passed through 0.45μm filtrating membrane.The obtained filtrate was injected with split ratio of 40∶1,and 10 photoinitiators were separated on DB-5 MS quartz capillary column(30 m×0.25 mm,2.5μm)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.