首页|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

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

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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0.05~2.0 μg·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.
Determination of 16 photoinitiator residuces in medicinal composite membranes with gas chromatography-mass spectrometry
Objective:To establish a gas chromatography-mass spectrometry(GC-MS)method for the determi-nation 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 0.05-2.0 μg·mL-1,and the correlation coefficients(r)were more than 0.997.The limits of detection(LODs)were 0.03 μg·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 0.02 μg·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.

gas chromatography-mass spectrometryphotoinitiatorsmedicinal composite membranesinternal standard methodresiduces

吴红洋

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重庆市食品药品检验检测研究院 国家药品监督管理局麻醉精神药品质量监测重点实验室,重庆 401121

气相色谱-质谱法 药用复合膜 光引发剂 内标法 残留量

重庆市绩效引导专项重庆市药品补充检验方法项目(2023)

CQIFDC-YJKT-2021-14

2024

药物分析杂志
中国药学会

药物分析杂志

CSTPCD北大核心
影响因子:1.039
ISSN:0254-1793
年,卷(期):2024.44(5)