GC-MS法快速测定铅笔涂层中18种光引发剂

Rapid determination of 18 photoinitiators in pencil coating by GC-MS

建立了快速测定铅笔涂层中18种光引发剂的气相色谱-质谱联用法(GC/MS)。样品以二氯甲烷为提取溶剂,在30℃温度下,超声提取30 min后,萃取液用100 mg N-丙基乙二胺(PSA)分散固相萃取净化,以气相色谱-质谱法(GC-MS)测定,外标法定量。18种光引发剂在0.2~4.0 mg/L(或0.1~4.0 mg/L)范围内线性良好,相关系数R^(2)均大于0.997,方法检出限(LODs)为0.4~1.0 mg/kg,定量限(LQDs)为1.0~2.0 mg/kg。3个加标水平(2.0或4.0、10.0和40.0 mg/kg)的回收率在75.2%~115.2%之间,相对标准偏差(RSDs)为1.0%~9.3%(n=6)。该方法可用于铅笔涂层中18种光引发剂含量的高通量检测。

A method was developed for the rapid determination of 18 photoinitiators in pencil coating by gas chromatography-mass spectrometer(GC-MS).The sample was extracted with dichloromethane at 30℃for30 minutes,then the extraction solution was purified by 100 mg primary secondary amine(PSA)dispersive solid phase extraction,determined by GC-MS and quantified by external standard method.The results showed that the method had good linearity in the range of 0.2-4.0 mg/L(or 0.1-4.0 mg/L),with the coefficient R^(2)>0.997.The limits of detection for the method were 0.4-1.0 mg/kg and the limits of quantitation(LOQs)were1.0-2.0 mg/kg.The recoveries of the three spiked levels(2.0 or 4.0,10.0 and 40.0 mg/kg)were between75.2%and 115.2%,and the relative standard deviations(RSDs)were between 1.0%and 9.3%(n=6).The method could be applied for the high-throughput determination of 18 photoinitiators in pencil coating.