色谱

色谱 ›› 2014, Vol. 32 ›› Issue (5): 513-518.DOI: 10.3724/SP.J.1123.2013.12023

• 技术与应用 • 上一篇    下一篇

液相色谱-串联质谱法测定面粉及其制品中的联二脲

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   

  1. 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
  • 收稿日期:2013-12-23 修回日期:2014-03-01 出版日期:2014-05-08 发布日期:2014-04-26
  • 通讯作者: 母昭德
  • 基金资助:

    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）.

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

WANG Ya1, WANG Junsu2, XIANG Lu1, XI Cunxian2, CHEN Dongdong3, PENG Tao3, WANG Guomin2, MU Zhaode1   

  1. 1. College of Pharmacy, Chongqing Medical University, Chongqing 400016, China;
    2. Chongqing Entry-Exit Inspection and Quarantine Bureau, Chongqing Engineering Technology Research Center of Import and Export Food Safety, Chongqing 400020, China;
    3. Chinese Academy of Inspection & Quarantine, Beijing 100123, China
  • Received:2013-12-23 Revised:2014-03-01 Online:2014-05-08 Published:2014-04-26

PDF

421

被引次数

17

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×2.0 mm，2.2 μm）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1~20000 μg/kg，相关系数为0.9999，定量限为5 μg/kg；当添加水平为5.0、10.0与50.0 μg/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。

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

Abstract:

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 permanganate. The azodicarbonamide was then derivatized using sodium p-toluene sulfinate solution. The separation was performed on a Shimpak XR-ODSⅡ column (150 mm×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 spectrometric detection was performed in multiple reaction monitoring (MRM) scan mode with a positive electrospray ionization (ESI+) source. The method used stable isotope internal standard quantitation. The calibration curve showed good linearity over the range of 1-20000 μg/kg(R2=0.9999). 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.

Key words: p-toluenesulfonyl semicarbazide, azodicarbonamide, biurea, derivatization, flour, flour products, liquid chromatography-tandem mass spectrometry (LC-MS/MS)

中图分类号: