Determination of alternaria mycotoxins in rapeseed oil by solid phase extraction with ultra high performance liquid chromatography-tandem mass spectrometry
  
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KeyWord:alternaria mycotoxins  solid phase extraction  ultra high performance liquid chromatography-tandem mass spectrometry  rapeseed oil
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LI Lei Guizhou Provincial Center for Disease Control and Prevention, Guiyang 550002, China
 
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Abstract:
      A method for analysis of alternaria mycotoxins in rapeseed oil was established by solid phase extraction with ultra high performance liquid chromatography- tandem mass spectrometry. The rapeseed oil was mixed with methanol and purified by Captive EMR-Lipid solid phase extraction column (3 mL, 300 mg). The purification liquid was collected and concentrated by nitrogen blowing. The alternaria mycotoxins were determined by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) and quantified by internal standard method. The purification capacity and eluent volume were optimized by investigating the recovery rate of alternaria mycotoxins. The results showed that the optimal purification capacity of rapeseed oil was 0.15 g, and the optimal eluent volume was 2.0 mL. The correlation coefficients of alternaria mycotoxins within linear range were greater than 0.998, and the recovery rates of alternaria mycotoxins ranged from 68.8% to 117.3% with the relative standard deviations of 8.6%-11.4%. The limit of detection and limit of quantification were 0.1-2.0 μg/kg and 0.3-6.0 μg/kg, respectively. The method had good sensitivity and recovery rate, and it was simple and easy to operate. The method was suitable for determination of alternaria mycotoxins in rapeseed oil.
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