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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 establish a method for the determination of 25 aromatic amines (PAAs) in polyurethane food contact materials in order to meet the international testing requirements of polyurethane plastic food contact materials and achieve accurate, rapid, economical and efficient determination of various aromatic amines. Methods The sample to be tested was immersed in 3% acetic acid solution (w / v), heated at 100 ℃ for 1 h, then 2 ml of the soaking solution was removed, then 0.06 g of KOH was added and vortexed for 1 min to pH 7.0. Add 0.5 g of NaCl, extracted with 2 ml of ethyl acetate for 1 min, and the supernatant was taken for GC-MS. Results 25 kinds of PAAs working curve r2 ≥ 0.991. The detection limit was 3μg / kg ~ 10μg / kg, the limit of quantification was 10μg / kg ~ 50μg / kg. In the blank samples, the spiked recoveries were tested at four spiked levels of 1, 3, 5 and 1.0 mg / kg for each aromatic amine. The spiked recoveries of each aromatic amine ranged from 80.3% 118.6%, RSD between 6.1% ~ 15.0%. Conclusion This method is simple, fast, accurate and reproducible. Provide technical support for the safety assessment of PAAs in food contact materials.