分散固相萃取-气相色谱法同时检测食品塑料 包装材料中7种烷基胺

Simultaneous determination of 7 kinds of alkylamines in food contact plastic package materials by gas chromatography coupled with dispersive solid-phase extraction

中文关键词:  烷基胺  分散固相萃取  食品塑料包装材料  气相色谱法

英文关键词:alkylamines  dispersive solid phase extraction  food contact plastic package materials  gas chromatography

中文摘要:

      目的 建立了分散固相萃取-气相色谱法(dispersive solid-phase extraction-gas chromatography, dSPE-GC)同时测定食品塑料包装材料中7种有机胺类物质的残留量。方法 样品经二氯甲烷超声萃取15 min, 采用25 mg C18、25 mg PSA和10 mg MWCNT固相萃取剂对提取液进行净化, 采用DB-1701色谱柱进行分离并进行气相色谱测定。同时对固相萃取剂的种类和用量、色谱柱等条件进行了优化。结果 7种烷基胺类物质在1.0~100 mg/L浓度范围内线性关系良好, 相关系数为0.9937~0.9996; 方法检出限为2.6~5.0 mg/kg; 添加水平为5.0、10.0和50 mg/kg时, 7种目标物的平均回收率为81.9%~107%, 日内精密度(n=6)为1.9%~5.3%; 日间精密度(n=5)为4.5%~9.1%。对市售10个塑料包装材料进行测定, 其中1个样品检出青霉胺, 含量为9.1 mg/kg。结论 本方法快速准确, 可适用于食品塑料包装材料中烷基胺类物质的测定。

英文摘要:

      Objective To establish a new method for the simultaneous determination of 7 kinds of alkylamines in food contact plastic package materials by gas chromatography coupled with dispersive solid phase extraction (dSPE-GC). Method The plastic sample was extracted with dichloromethane by ultrasonication for 15 min, and purified with solid phase extractant including 25 mg C18, 25 mg PSA and 10 mg MWCNT. Then the extract was separated by column of DB-1701 and determined by gas chromatography. Meanwhile, the type of extraction solvent, clean-up sorbent and column were optimized. Result Seven kinds of alkylamines had a good linear relationship in the range of 1.0~100 mg/L with correlation coefficient of 0.9937~0.9996, the limit of detection was ranged from 2.6 mg/kg to 5.0 mg/kg. The mean recoveries spiked at 3 levels of 5.0,10.0和50 mg/kg were in the range of 81.9%~107%. The precision was 1.9%~5.3% (n=6), and the inter-precision was 4.5%~9.1% (n=5). Ten plastic packaging materials were tested for penicillamine, and only one was found positive and the concentration was 9.1 mg/kg. Conclusion The method is rapid and accurate, which can be used for determination of alkylamines compounds in food contact plastic packaging materials.