Determination of semicarbazide in flour and flour products by SPE purification ultra-high performance liquid chromatography-tandem triple quadruple mass spectrometry
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(Key Laboratory of Food Safety Risk Assessment of Ministry of Health,China National Center For Food Safety Risk Assessment,Beijing 100021,China)

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    Abstract:

    An ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry (UPLC-MS/MS) method was developed for the determination of emicarbazide (SEM) in flour and flour products.MethodsStable isotope labeled internal standard was added to the sample and SEM reacted with o-nitrobenzaldehyde in 0.2 mol/L HCl to produce stable derivatization. The derivatization was cleaned up with HLB SPE cartridge, eluted with ethyl acetate, dried with nitrogen, and redissolved with 0.1% formic acid. The sample was separated on a waters BEH C18 column. The detection was performed with waters Xevo TQ-S using postive electrospray ionization mode and multiple-reaction monitoring mode. ResultsThe results showed that the linear range for SEM was 0.5-100 μg/kg in flour. The method showed good accuracy with RSD<20% (n=6) and recovery in between 60% to 120%.ConclusionThis method is fast, simple and has good reproducibility. It is suitable for semicarbazide determination in flour and flour products.

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WANG Dan, CHEN Ying, SONG Shu-feng, GAO Jie, LIANG Jiang, ZHAO Yun-feng. Determination of semicarbazide in flour and flour products by SPE purification ultra-high performance liquid chromatography-tandem triple quadruple mass spectrometry[J].中国食品卫生杂志,2014,26(6):579-583.

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  • Received:June 30,2014
  • Revised:
  • Adopted:
  • Online: December 19,2014
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