液相色谱-串联质谱法测定面粉及其制品中的联二脲  

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

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

机构地区：[1]重庆医科大学药学院,重庆400016 [2]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 [3]中国检验检疫科学研究院,北京100123

出　　处：《色谱》2014年第5期513-518,共6页Chinese Journal of Chromatography

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)

摘　　要：建立了面粉及其制品中联二脲的液相色谱-串联质谱（ LC-MS/MS）测定及确证方法。采用纯水振荡提取样品中的联二脲，联二脲经高锰酸钾氧化后，转变为偶氮甲酰胺，再加入对甲苯亚磺酸钠使偶氮甲酰胺衍生为对甲苯磺酰氨基脲。以乙腈和2 mmol/L乙酸铵溶液（含0.2％（ v/v）甲酸）为流动相进行梯度洗脱，经 Shimpak XR-ODSⅡ色谱柱（150 mm＆#215;2.0 mm，2.2μm）分离，电喷雾正离子模式电离（ESI＋），多反应监测（MRM）模式检测，同位素内标法定量。方法的线性范围为1~20000μg/kg，相关系数为0.9999，定量限为5μg/kg；当添加水平为5.0、10.0与50.0μg/kg时，联二脲的平均回收率为78.3％~108.0％，相对标准偏差（ RSDs）不大于5.73％。本方法新颖、可靠、灵敏、线性范围广，而且实用性强，可用于面粉及其多种制品中联二脲的测定和确证。A novel method was established for the determination and identification of biurea in flour and its products using liquid chromatography-tandem mass spectrometry（ LC-MS/MS）. The biurea was extracted with water and oxidized to azodicarbonamide by potassium permanga-nate. The azodicarbonamide was then derivatized using sodium p-toluene sulfinate solution. The separation was performed on a Shimpak XR-ODSⅡ column（150 mm＆#215;2. 0 mm,2. 2 μm）using the mobile phase composed of acetonitrile and 2 mmol/L ammonium acetate aqueous solution （containing 0. 2%（v/v）formic acid）with a gradient elution program. Tandem mass spectro-metric detection was performed in multiple reaction monitoring（ MRM）scan mode with a posi-tive electrospray ionization（ ESI＋）source. The method used stable isotope internal standard quantitation. The calibration curve showed good linearity over the range of 1-20 000 μg/kg（ R 2=0. 999 9）. The limit of quantification was 5 μg/kg for biurea spiked in flour and its products. At the spiking levels of 5. 0,10. 0 and 50. 0 μg/kg in different matrices,the average recovery of biurea was 78. 3%-108. 0% with the relative standard deviations（ RSDs）≤5. 73%. The method developed is novel,reliable and sensitive with wide linear range,and can be used to determine the biurea in flour and its products.

关 键 词：液相色谱-串联质谱法 衍生 联二脲 面粉 面制品 偶氮甲酰胺 对甲苯磺酰氨基脲 

分 类 号：O658[理学—分析化学]