面粉中氨基脲含量的测定及偶氮甲酰胺和氨基脲转化规律的研究

Study on the determination of semicarbazide in flour products and transformation law between azodicarbazide and semicarbazide

中文关键词:  面制品  偶氮甲酰胺  氨基脲  超高效液相色谱-串联质谱法

英文关键词:flour product  azodicarbazide  semicarbazide  ultra high performance liquid chromatography-tandam mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-串联质谱法测定面制品中的氨基脲含量, 并研究偶氮甲酰胺添加水平对面粉中氨基脲含量的影响及两者的转化条件。方法 样品经盐酸水解、邻硝基苯甲醛衍生、HLB小柱净化及乙酸乙酯提取; 质谱以电喷雾电离源正离子模式扫描监测, 用带有同位素内标的衍生物15N213C-SEM-NBA定量检测目标氨基脲衍生物。结果 氨基脲在0.5~100 μg/kg范围内呈良好线性关系, 相关系数为0.9995, 检出限为0.5 μg/kg, 加标回收率在85.1%~114.6%之间, 相对标准偏差为3.2%~6.9%。市售10份面制品中氨基脲的阳性检出率为41.7%。氨基脲是偶氮甲酰胺在湿热的条件下生成的, 并且同一种面制品中外部氨基脲含量比内部含量大。结论 本方法快速、准确且灵敏度高, 可适用于面制品中氨基脲的定量分析。

英文摘要:

      Objective To establish a method for the determination of semicarbazide(SEM) residues in flour products by ultra high performance liquid chromatography-tandam mass spectrometry, and also study the effect of azodicarbazide(ADA) adding levels on the semicarbazide content in the bread and their transform condition. Methods Samples were hydrolyzed with hydrochloric acid, derivated by nitrobenzaldehyde(2-NBA), cleaned by HLB column, and extracted with ethyl acetate. Mass spectrometer was used by electrospray ionization source positive iron mode for scanning monitoring, and then the target of semicarbazide derivatives was quantified with isotope internal standard of 15N213C-SEM-NBA. Results SEM had a good linear relationship in the range of 0.5~100 μg/kg with the correlation coefficient of 0.9995, the limit of detection was 0.5 μg/kg. The recoveries was 85.1%~114.6% and RSD was 3.2%~6.9%. The positive percentage of semicarbazide in the ten commercial bread was 41.7%. ADA can transform to SEM under the hot and damp condition, and the SEM content of surface was higher than that of inside in the same bread. Conclusion The method is rapid, precise and sensitive, which is suitable for the quantitative analysis of semicarbazide in flour product.