气相色谱-质谱法测定药用复合膜中16种光引发剂的残留量

Determination of 16 photoinitiator residuces in medicinal composite membranes with gas chromatography-mass spectrometry

目的:建立气相色谱-质谱法同时测定药用复合膜中二苯甲酮、4-甲基二苯甲酮等16种光引发剂的残留量。方法:样品经乙酸乙酯超声提取后,采用TR-5MS气相色谱柱,程序升温;质谱检测器:电子轰击源,正离子模式,选择反应监测模式下进行分析,内标法定量。结果:16种光引发剂在0.05~2.0μg·mL^(-1)范围内线性关系良好,r均>0.997,检测限均为0.03μg·mL^(-1),平均回收率(n=6)在81.3%~94.0%,RSD为2.1%~6.2%。10批次药用复合膜中光引发剂4-ITX检出率为30%,最高含量为0.02μg·cm^(-2)。结论:该方法前处理简单,灵敏度高,结果准确,可用于药用复合膜中多种光引发剂残留量的同时测定。

Objective:To establish a gas chromatography-mass spectrometry(GC-MS)method for the determination of 16 photoinitiator residuce levels in medicinal composite membranes,including benzophenone(BP)and 4-methylbenzophenone(4-MBP).Methods:The samples were extracted by ethylacetate,separated with TR-5MS column.The mass spectrum was analyzed with EI ionization,positive ion mode and selective reaction monitoring(SRM)mode and quantified with internal standard method.Results:The 16 kinds of photoinitiators had good linear relationships in the range of 0.05-2.0μg·mL^(-1),and the correlation coefficients(r)were more than 0.997.The limits of detection(LODs)were 0.03μg·mL^(-1).The average recoveries were(n=6)ranged from 81.3%to 94.0%,with RSDs of 2.1%-6.2%.The detection rate of 4-Isopropylthioxanthone(4-ITX)in the medicinal composite membranes was 30%,and the highest content was 0.02μg·cm^(-2).Conclusion:The method is accurate with high sensitivity and simple pretreatment,which can be used for the detecting the kinds of photoinitiators in medicinal composite membranes.