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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 C_(18)、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。
OBJECTIVE To establish a dispersive solid-phase extraction-gas chromatography (dSPE-GC) for the simultaneous determination of 7 organic amines residues in food plastic packaging materials. Methods The samples were extracted by dichloromethane for 15 min. The extracts were purified by 25 mg C 18, 25 mg PSA and 10 mg MWCNT SPE. The extracts were separated by gas chromatography on a DB-1701 column. At the same time, the type and amount of solid phase extraction agent, column and other conditions were optimized. Results The linearity of seven alkylamines ranged from 1.0 to 100 mg / L. The correlation coefficients ranged from 0.9937 to 0.9996. The detection limits were 2.6-5.0 mg / kg. The addition levels were 5.0, 10.0 and 50 mg / kg, the average recoveries of the seven target species ranged from 81.9% to 107%, intra-day precision (n = 6) was 1.9% to 5.3%, and daytime precision (n = 5) was 4.5% to 9.1%. On the market of 10 plastic packaging materials were measured, including a sample of penicillamine, the content of 9.1 mg / kg. Conclusion The method is rapid and accurate and can be applied to the determination of alkylamines in food plastic packaging materials.