顶空气相色谱-质谱联用法测定高密度聚乙烯瓶垫及瓶身中的溶剂残留  

Determination of residual solvents in HDPE bottle cushion and bottle body by headspace gas chromatography-mass spectrometry

作　　者：刘生彩 刘柏龙 夏巧红 杜浩 宋平顺 LIU Shengcai;LIU Bailong;XIA Qiaohong;DU Hao;SONG Pingshun(Gansu Institute of Drug Control,Lanzhou 730070,China)

机构地区：[1]甘肃省药品检验研究院,兰州730070

出　　处：《中国药品标准》2021年第4期302-308,共7页Drug Standards of China

基　　金：2019年甘肃省药品监督管理局项目,课题编号:2019GSMPA022。

摘　　要：目的:采用气相色谱-质谱联用(GC-MS)确定样品中的未知峰,建立顶空-气相色谱法(HS-GC)检测口服固体高密度聚乙烯瓶及药用聚酯·铝·聚乙烯封口垫片中溶剂残留量的方法。方法:样品顶空平衡条件为110℃,60 min,分流进样;进样口温度180℃;柱温为程序升温:初始温度30℃,保持35 min,以50℃·min^(-1)速率升温至80℃,保持20 min,再以100℃·min^(-1)速率升温至200℃,保持1 min;检测器为FID,温度250℃。结果:15种有机溶剂的线性范围在0.007~6.000 mg·m^(-2),相关系数r均大于0.99;方法检出限为0.0013~0.0122 mg·m^(-2),定量限为0.0034~0.0305 mg·m^(-2),RSD为0.001%~0.054%(n=5)。结论:表明仪器灵敏度高,方法稳定,操作简单,能够快速、有效的监控产品中的残留溶剂的含量,为提高产品质量提供参考依据。Objective:To determine the unknown peaks in the samples by gas chromatography-mass spectrometry(GC-MS)and establish an headspace gas chromatography(HS-GC)method for determination of residual solvents in high density polyethylene(HDPE)bottles for oral solid preparation and foil laminated closure liners(PET/AL/PE)for pharmaceutical packaging.Methods:The headspace equilibrium condition was 110℃for 60 min,the split injection was adopted,and the injection port temperature was 180℃.The programmed temperature procedure was as follows:maintaining the initial temperature 30℃for 35 min,raising to 80℃at a rate of 50℃·min^(-1) and keeping it for 20 min,then raising to 200℃at a rate of 100℃·min^(-1) and keeping it for 1 min.FID detection was adopted and the detection temperature was 250℃.Results:The results showed that the linear ranges of 15 organic solvents fell into 0.007-6.0 mg·m^(-2) with correlation coefficients r more than 0.99.The limits of detection was 0.0013-0.0122 mg·m^(-2),and the limits of quantification was 0.0034-0.0305 mg·m^(-2) with RSDs as 0.001%-0.054%(n=5).Conclusion:The instrument has the high sensitivity.The established method is stable and simple,and it can quickly and effectively determine the contents of residual solvents in the products,and provide reference for improving the quality of products.

关 键 词：顶空 气相色谱-质谱联用 溶剂残留 药品包装材料 YBB系列标准 

分 类 号：R921.2[医药卫生—药学]