微波萃取-气相色谱质谱联用法测定快递包装塑料中的12种邻苯二甲酸酯
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摘要
本文建立了微波萃取-气相色谱质谱联用法(GC-MS)测定快递包装塑料中的12种邻苯二甲酸酯。样品粉碎后加入15 mL乙酸乙酯,用微波萃取仪100℃下萃取30 min,萃取液加入内标后定容,用0.45μm的滤膜过滤,滤液经DB-5MS色谱柱分离,供GC-MS分析。质谱采用电子轰击电离源(electron impact ion source,EI)和选择离子监测模式(selected ion monitor,SIM),以内标法定量。DMP,DEP,DPRP,DIBP,DBP,DHxP,BBP,DCHP,DEHP和DNOP的方法检出限为0.00125%,DINP,DIDP方法检出限为0.0125%。DINP,DIDP在2.5～100 mg/L,其余10种物质在0.25～10mg/L范围内线性良好,线性相关系数R2均大于0.9995。12种邻苯二甲酸酯的平均回收率为90.3～104.9%,精密度RSD为1.1%～5.8%。该方法简便、快速、准确,可应用于快递包装塑料中邻苯二甲酸酯的检测。
In this paper a method for determination of 12 kinds of phthalate esters(PAEs)in express plastic packaging materials by microwave extraction-gas chromatography-mass spectrometry was established. The samples were smashed, and then added 15 mL ethyl acetate, microwave extracting for 30 min at 100 ℃.After filtration with 0.45 μm filter membrane the extracted solution was separated by DB-5 MS column and detected by GC-MS.The determination was performed in electron impact ion source(EI)and selected ion monitoring(SIM)mode with internal standard method for quantitative analysis. The limits of method detection(MDL)of DMP,DEP,DPRP,DIBP,DBP,DHxP,BBP,DCHP,DEHP,DNOP were 0.00125%,and DINP,DIDP were 0.0125%.Twelve kinds of PAEs had good linear relationship in the range of 0.25 ～10 mg/L(DMP,DEP,DPRP,DIBP,DBP,DHxP,BBP,DCHP,DEHP,DNOP),2.5-100 mg/L(DINP,DIDP)with the correlation coefficients greater than0.9995.The recovery rates were in the range of 90.3%-104.9%with the relative standard deviation(RSD)of 1.1%-5.8%.The method is simple,rapid and accurate, which can be applied in the determination of twelve kinds of PAEs in express plastic packaging materials.
In this paper a method for determination of 12 kinds of phthalate esters(PAEs)in express plastic packaging materials by microwave extraction-gas chromatography-mass spectrometry was established. The samples were smashed, and then added 15 mL ethyl acetate, microwave extracting for 30 min at 100 ℃.After filtration with 0.45 μm filter membrane the extracted solution was separated by DB-5 MS column and detected by GC-MS.The determination was performed in electron impact ion source(EI)and selected ion monitoring(SIM)mode with internal standard method for quantitative analysis. The limits of method detection(MDL)of DMP,DEP,DPRP,DIBP,DBP,DHxP,BBP,DCHP,DEHP,DNOP were 0.00125%,and DINP,DIDP were 0.0125%.Twelve kinds of PAEs had good linear relationship in the range of 0.25 ～10 mg/L(DMP,DEP,DPRP,DIBP,DBP,DHxP,BBP,DCHP,DEHP,DNOP),2.5-100 mg/L(DINP,DIDP)with the correlation coefficients greater than0.9995.The recovery rates were in the range of 90.3%-104.9%with the relative standard deviation(RSD)of 1.1%-5.8%.The method is simple,rapid and accurate, which can be applied in the determination of twelve kinds of PAEs in express plastic packaging materials.
引文
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[4]孙春峰,秦芳.化妆品塑料包装中邻苯二甲酸酯含量的测定[J].塑料工业,2018,46(1):95-98.
[5]步召胜.食品塑料包装材料中邻苯二甲酸酯含量的测定[J].塑料工业,2017,45(5):96-98.