顶空气相色谱-质谱法测定药品包装材料中40种有机溶剂残留量  

Simultaneous determination of 40 kinds of residual organic solvents in pharmaceutical packaging materials by headspace gas chromatography-mass spectrometry

作　　者：付蒙 陈晓莉 周姝 江燕 FU Meng;CHEN Xiaoli;ZHOU Shu;JIANG Yan(Hubei Institute for Drug Control,Hubei engineering Research Center for Drug Quality Control,NMPA key laboratory of Traditional Chinese medicine,Wuhan 430075,China)

机构地区：[1]湖北省药品监督检验研究院,湖北省药品质量检测与控制工程技术研究中心,国家药品监督管理局中药质量控制重点实验室,武汉430075

出　　处：《中国药品标准》2023年第1期96-103,共8页Drug Standards of China

基　　金：湖北省药品监督管理局科研项目(项目编号:20200108)。

摘　　要：目的:建立测定药品包装材料中正辛烷、丙酮、辛烯、乙酸乙酯等40种有机溶剂残留量的方法。方法:采用顶空气相色谱-质谱法,色谱条件为Agilent VF-WAX MS毛细管气相色谱柱(60 m×0.32 mm,1.00μm),柱温为程序升温(起始温度45℃,保持5 min,以5℃·min^(-1)升温至150℃,再以20℃·min^(-1)升温至220℃,保持4 min),进样口温度:220℃;载气为高纯氦气,流速为1.0 mL·min^(-1),分流比为10∶1;进样体积为1 mL;质谱条件为电子轰击离子源(EI),轰击电压70 eV;离子源温度为280℃,接口温度250℃;扫描方式:定性SCAN(质量数范围29~650),定量SIM。结果:所建立的方法呈良好的线性关系,相关系数r为0.9953~0.9996,各有机溶剂平均回收率均在94.25%~107.46%范围内,RSD为0.06%~1.92%。药用复合膜、药用复合硬片、药用铝箔的有机溶剂残留量检测结果分别为0.011~1.688、2.631~24.586、0.084~18.663 mg·m^(-2)。结论:本法适用于药品包装材料中有机溶剂残留量的检测。Objective:To establish a method for the determination of 40 kinds of residual organic solvents,such as n-octane,acetone,octene and ethyl acetate in pharmaceutical packaging materials.Methods:A headspace gas chromatography-mass spectrometry(GC-MS-RRB-method was developed with Agilentlent VF-WAX MS capillary column(60 m×0.32 mm,1.00μm),the column temperature was a programmed temperature rise(starting temperature 45℃,holding for 5 min,5℃·min^(-1) to 150℃,then 20℃·min^(-1) to 220℃,holding for 4 min),the sample inlet temperature was 220℃,the carrier gas was high purity helium,the flow rate was 1.0 mL·min^(-1),the split ratio was 10∶1,the volume of sample injection was 1 mL,the condition of mass spectrometry was electron bombardment ion source(EI),the bombardment voltage was 70 eV,the temperature of ion source was 280℃,the interface temperature was 250℃,scanning mode:qualitative SCAN(quality number range 29-650),quantitative SIM.Results:The correlation coefficient(r)was 0.9953-0.9996.The average recovery of each organic solvent was in the range of 94.25%-107.46%.The RSD was 0.06%-1.92%.The detection results of residual organic solvents in compound film,hard tablet and aluminum foil were 0.011-1.688,2.631-24.586 and 0.084-18.663 mg·m^(-2),respectively.Conclusion:This method is suitable for the determination of residual organic solvents in pharmaceutical packaging materials.

关 键 词：顶空气相色谱-质谱法 药品包装材料 药用复合膜 药用铝箔 药用复合硬片 有机溶剂 残留量 

分 类 号：R921.2[医药卫生—药学]