液相色谱-串联质谱研究面粉及其制品中偶氮甲酰胺降解规律及氨基脲污染水平  

Determination of semicarbazide in flour and flour products by liquid chromatography-tandem mass spectrometry

作　　者：周启明[1] 向露[2] 王俊苏[1] 郗存显[1] 王雅[2] 彭涛[3] 母昭德[2] 王国民[1] 

机构地区：[1]重庆出入境检验检疫局,重庆市进出口食品安全工程技术研究中心,重庆400020 [2]重庆医科大学,重庆400016 [3]中国检验检疫科学研究院,北京100123

出　　处：《分析试验室》2014年第7期782-786,共5页Chinese Journal of Analysis Laboratory

基　　金：国家质检公益性行业科研专项基金(201210016;201210086);国家"十二五"科技支撑计划项目(2012BAD33B02;2012BAK08B01)资助

摘　　要：建立了面粉及其制品中氨基脲的液相色谱-串联质谱（LC-MS/MS）测定方法,并研究了面粉及其制品中偶氮甲酰胺降解规律及氨基脲污染水平。面粉及其制品等经0.1 mol/L HCl溶液水解,邻硝基苯甲醛衍生化,乙酸乙酯提取,正己烷脱脂后,采用LC-MS/MS测定,内标法定量。氨基脲的线性范围为0.5～100μg/L;在面粉、馒头、面包等基质中添加浓度为0.5,1.0,5.0μg/kg时,氨基脲回收率范围为89.0%～99.4%,相对标准偏差在4.8%～12%之间;氨基脲定量限为0.5μg/kg。面粉制品中氨基脲的含量与偶氮甲酰胺的添加量呈线性关系。市售面包中氨基脲的阳性检出率为92.0%,阳性样品中氨基脲污染水平为17.6～353.0μg/kg,表明目前我国面包制品中氨基脲污染状况较为严重。A method for the determination of semicarbazide in flour and its products was developed,and the degradation pattern of azodicarbazide and contamination level of semicarbazide were studied.Samples were hydrolyzed by 0.1 N hydrochloric acid and derivatized with o-nitrobenzaldehyde.The resultant derivative was extracted with ethyl acetate,and the lipid was removed by liquid-liquid extraction using n-hexane.The target compound was detected by LC-MS/MS and quantification was performed based on an internal standard.Good linearity of semicarbazide was achieved over the concentrations range of 0.5 μg/L ～ 100 μg/L,and the recoveries of semicarbazide in flour,steamed bun and bread fortified at the three spiking levels of 0.5,1.0,5.0μg/kg were 88.8% ～ 99.4 % with relative standard deviations of 4.8% ～ 11.5 %.The limit of quantification was 0.5 μg/kg.The method is reliable and reproducible,and could be used for the determination of semicarbazide in flour and its products.The contents of semicarbazide in bread show good linearity with azodicarbazide concentrations in flour.Concentrations of semicarbazide in commercial positive bread were from17.6 μg/kg to 353.0 μg/kg with positive percentage of 92.0 %,which indicates that the situation of semicarbazide contamination is serious in our country.

关 键 词：氨基脲 面粉 面粉制品 液相色谱-串联质谱 偶氮甲酰胺 污染水平 

分 类 号：O657.63[理学—分析化学]