Determination of 5 Fusarium Mycotoxins in Wheat Flour by QuEChERS Extraction Combined with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
  
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KeyWord:ultra performance liquid chromatography-tandem mass
  
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YANG Jun,SUN Xiao-jie,HU Wen-yan,WANG Yu-mei 南京市食品药品监督检验院
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Abstract:
      An ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was developed for the simultaneous determination of 5 fusarium mycotoxins in wheat flour,including enniatins A,enniatins A1,enniatins B,enniatins B1 and beauvericin.The fusarium mycotoxins were extracted from the samples using a modified QuEChERS-based extraction procedure without any further clean-up step.The separation of the analytes was carried out on an Agilent Eclipse Plus C18 column(50 mm×2.1 mm,1.8 μm) using the mobile phases of methanol and 2 mmol/L ammonium acetate by gradient elution.The detection was performed in the electrospray ion(ESI) positive mode and multiple reaction monitoring(MRM) mode.The matrix-matched calibrations were used to quantify the residue concentrations.The proposed method showed good linear relationship with correlation coefficients all above 0.993.The limits of detection(LODs)were in the range of 0.3-0.8 μg/kg,and the limits of quantitation(LOQs) were 0.8-2.4 μg/kg.The blank samples were fortified at three spiked levels(1 times,2 times,10 times of LOQ),and the average recoveries ranged from 74.0% to 85.4% with relative standard deviations(RSDs) of 5.6%-13.1%.The developed method was successfully applied in analysis of fusarium mycotoxins in 30 samples bought from the market.The method was simple,rapid,accurate and sensitive,and was suitable for the simultaneous analysis of multi-fusarium mycotoxins in wheat flour.
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