[Determination of deoxynivalenol in grain and its products by solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry].

A method was established for the determination of deoxynivalenol(vomitoxin) in grain and its products based on solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The sample was firstly extracted by acetonitrile-water(84∶16,v/v).The extract was then cleaned-up by an HLB solid phase extraction cartridge.The separation was carried out on a Phenomenex Kinetex C18 column(100 mm×4.6 mm,2.6μm) with a gradient elution using 0.3‰ ammonia solution-acetonitrile as mobile phases.The analysis of deoxynivalenol was performed under electrospray negative ionization mode.The limit of detection(LOD,S/N=3) and the limit of quantification(LOQ,S/N=10) were 20 μg/kg and 50 μg/kg,respectively.A good linearity(r0.99) was achieved for the target compound over the range of 20-1 000 μg/L.The recoveries at the three spiked levels(50,100,500 μg/kg) in the blank matrices such as flour,barley,soybean,rice,cornmeal,cassava and wheat,were varied from 75.6% to 111.0% with the relative standard deviations no more than 13.0%.The method is accurate,efficient,sensitive and practical.The cost of pretreatment is obviously reduced by replacing immunoaffinity columns and Mycosep columns with HLB columns which have the same purification effect.