Citation: WANG Ya, WANG Junsu, XIANG Lu, XI Cunxian, CHEN Dongdong, PENG Tao, WANG Guomin, MU Zhaode. Determination of biurea in flour and its products by liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(5): 513-518. doi: 10.3724/SP.J.1123.2013.12023 shu

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

WANG Ya ¹ ,
WANG Junsu ² ,
XIANG Lu ¹ ,
XI Cunxian ² ,
CHEN Dongdong ³ ,
PENG Tao ³ ,
WANG Guomin ² ,
MU Zhaode ^1,,

1.
1. College of Pharmacy, Chongqing Medical University, Chongqing 400016, China;

Corresponding author: MU Zhaode,
Received Date: 23 December 2013
Available Online: 1 March 2014
Fund Project: 国家质检公益性行业科研专项基金(201210016,201210086) (201210016,201210086)国家“十二五”科技支撑计划项目(2012BAD33B02,2012BAK08B01). (2012BAD33B02,2012BAK08B01)

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