液相色谱串联质谱法测定面粉熟食制品中的氨基脲  

Determination of Semicarbazide in Flour Cooked Food Products by Liquid Chromatography-Electrospray Tandem Mass Spectrometry

作　　者：刘琴芳[1] 

机构地区：[1]安徽国家农业标准化与监测中心,国家农副加工食品质量监督检验中心,安徽合肥230051

出　　处：《安徽化工》2013年第5期79-81,共3页Anhui Chemical Industry

摘　　要：建立了一种麦面熟食制品中氨基脲的液相色谱-串联质谱（HPLC-MS/MS）检测方法.面粉熟食样品在40℃水浴超声下经盐酸水解,邻硝基苯甲醛快速衍生化,乙酸乙酯提取,浓缩净化后,采用HPLC-ESI-MS/MS检测分析,在多反应监测模式（MRM）下,外标法定量.在0.25～10μg/kg范围内标准曲线的相关系数大于0.998.在不同添加水平下的回收率为95.5％～101.1％,定量限（LOQ）为1μg/kg,检出限（LOD）为0.25μg/kg.该方法准确、灵敏,达到了检测面粉熟食制品中氨基脲的检测要求.A determination method has been developed for the analysis of semicarbazide in flour cooked food products by liquid chromatography-electrospray ionization tandem mass spectrometry. Samples were hydrolyzed with dilute hydrochloric acid, derivatied with 2-nitrobenzene formaldehyde, extracted by ethyl acetate, then cleaned up, and ultimately adopted LC-ESI-MS/MS method for qualitative and quantitative analysis. Four nitrofuran metabolites can be seperated with a gradient of acetonitrile and 0.05% formic acid in 30 mintues. The calibration graphs were linear from 0.25 to 10 μ g/kg, and correlation coefficients r〉0.998. The average recoveries were from 95.5% -101.1% in different spike levels . Limits of quantification （LOQ） and limits of detection （LOD） were 1 μ g/kg and 0.25 μ g/kg. The method is simple, efficient, sensitive, accurate and can meet the requirements of determination for semicarbazide in flour cooked food products.

关 键 词：氨基脲 面粉熟食制品 高效液相色谱 质谱法 

分 类 号：O657.72[理学—分析化学]