摘要
目的为满足国际关于聚氨酯塑料食品接触材料的检测限量要求,同时实现准确、快速、经济、高效地测定多种芳香胺而建立聚氨酯类食品接触材料中25种芳香胺(PAAs)的检测方法。方法将待测样品浸入3%乙酸溶液(w/v)中,在100℃下加热1 h后,移取2 ml浸泡液,再加入KOH 0.06 g,涡旋振荡1 min,至pH=7.0,加入0.5 g NaCl,以2 ml乙酸乙酯萃取1 min,取上清液进GC-MS检测。结果 25种PAAs工作曲线的r2≥0.991。方法检出限为3μg/kg^10μg/kg,定量限为10μg/kg^50μg/kg。在空白样品中,以各芳香胺定量限的1倍、3倍、5倍及1.0 mg/kg的4个加标水平进行加标回收率测试,各芳香胺的加标回收率在80.3%~118.6%之间,RSD在6.1%~15.0%之间。结论本方法具有简便快捷、定量准确及重现性好等特点。为实现对食品接触材料中PAAs的安全性评价提供技术支持。
Objective To develop a rapid,accurate,economic and high-efficiency method for determination of 25 primary aromatic amines（PAAs） in polyurethane food contact materials by gas chromatography-mass spectrometry,in order to meet the international requirements of quantitative detection of polyurethane plastic food contact materials.Methods The sample was immersed into 3% acetic acid（w /v） and then heated for 1 h under 100 ℃.Then 2 ml immersion was transferred and adjusted the pH to 7.0 by 0.06 g KOH,then 0.5 g NaCl was added into the immersion.Finally the immersion was extracted by 2 ml ethyl acetate for 1 min.The supernatant was determinated by GC-MS.Results The calibration curves of 25 kinds of PAAs obtained were linear with correlation coefficients greater than 0.991.The limit of detection was 3 μg /kg - 10 μg /kg and the limit of quantification were 10 μg /kg - 50 μg /kg.The spiked concentrations were 1,3 times and 5 times as the quantitation limits of various aromatic amine and 1.0 mg /kg.The recoveries of the aromatic amine were 80.3% - 118.6% and the RSDs were 6.1% - 15.0% at the four spiked levels.Conclusion The method has the advantages of convenience,accurate quantification and good reproducibility.It has provided methodological foundation for safety evaluation of PAAs in food contact materials.
出处
《中国卫生检验杂志》
北大核心
2014年第11期1532-1535,1539,共5页
Chinese Journal of Health Laboratory Technology
关键词
聚氨酯
食品模拟介质
芳香胺气
气相色谱-质谱法
定性定量分析
Polyurethane
Food simulates
Aromatic amines
Gas chromatography-mass spectrometry
Qualitative and quantitative analysis
