Determination of Semicarbazide in Flour Products by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry
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Abstract:
A method was developed for the determination of semicarbazide in flour products based on solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS ) in the article．The samples were homogenized with 0.2mol/L HCl, derivatized with 2-notrobenzaldehyde, and the derivative was extracted with ethyl acetate. The extract was cleaned up by a solid phase extraction cartridge. The target analytes were separated on a UPLC BEH C18 column with gradient elution using acetonitrile and water containing 0.1% (V/V) formic acid as mobile phase. The identification and quantification were achieved by using ESI-MS/MS in positive ion mode and with multiple reactions monitoring (MRM). The linear range was from 1 to 100 μg /kg with the correlation coefficient r=0.9993 for semicarbazide. The limit of detection (LOD) was 0.4 μg/kg. The recoveries of the method were ranged from 85.8% to 112.6% at the spiked levels of 2, 10, 50μg /kg and the relative standard deviation was less than 9%. The method was suitable for the qualitative and quantitative of semicarbazide in different flour products.
