超高效液相色谱串联质谱法-柱前衍生同时测定食品接触产品中的5种异氰酸酯

Simultaneous determination of 5 kinds of isocyanates in food contact materials by ultra performance liquid chromatography-tandem mass spectrometry with pre-column derivatization

中文关键词:  超高效液相色谱-串联质谱法  衍生法  食品接触材料  异氰酸酯

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  pre-column derivation  food contact materials  isocyanates

中文摘要:

      目的 建立超高效液相色谱-串联质谱法-柱前衍生同时测定食品接触材料中5种异氰酸酯的迁移物的检测方法。方法 样品经二氯甲烷提取, 利用二正丁胺(di-n-butylamine, DBA)进行柱前衍生, 氮气浓缩后乙腈复溶。结果 5种异氰酸酯衍生物在1~100 μg/L范围内线性良好, 相关系数r在0.9990~0.9994之间。5种异氰酸酯3个添加水平下回收率在93.5%~109.6%之间, RSD(n=6)均在8.94%以下, 检出限与定量限分别为0.05~0.2 μg/L、0.2~0.5 μg/L。结论 本方法灵敏度高, 重复性好, 可应用于5种异氰酸酯日常检测工作。

英文摘要:

      Objective To establish a method for simultaneous determination of 5 kinds of isocyanates in food contact materials of migration test methods by ultra performance liquid chromatography-tandem mass spectrometry with pre-column derivatization. Methods The samples were extracted with dichloromethane, derivatized with di-n-butylamine (DBA) and finally concentrated by nitrogen and dissolved with acetonitrile. Results The 5 isocyanate derivatives had good linear relationships in the range of 1~100 μg/L, and the correlation coefficients were 0.9990~0.9994. The recoveries of 5 isocyanate derivatives at 3 different spiked levels were 93.5%~109.6%, with the relative standard deviations of below 8.94%(n=6). The limits of detection were 0.05~0.2 μg/L and the limits of quantitation were 0.2~0.5 μg/L. Conclusion This method has high sensitivity and repeatability, which can be used in daily test of 5 kinds of isocyanates.