The Study Of The Methods For The Determination Of Three Major Fusarium Mycotoxins In Formula Feed

GC-MS and HPLC-MS were studied and applied to determinate DON, NIV and ZEA in formula feed. The conditions of extraction, derivation and instrument have been optimized.The DON and NIV in feed are extracted with 100ml acetonitrile-water (84:16, V/V), vibrating for 60 min, then cleaned-up by Mycosep?227.The method of determination of DON and NIV by GC-MS is used HFBI as derivatization reagent, the toxins are derivatived at 70℃for 50min, or used TMSI-BSA-TMCS (3:3:2, V/V/V) as derivatization reagent, derivatived at room temperature for 15min. After seperated by HP-5 MS columnSpecific ions are used for qualitative analysis, extracted ions for quantitative analysis. The extracted ion of fluoroacylation for DON is 294 and for NIV is 333, the extracted ions of trimethylsilylation for DON and NIV are 422 and 379 respectively.The detection limit of the method of determination after fluoroacylation is 3ng/g, RSD≤9.0%. The recoveries of DON and NIV added to feed at the range of 20～700ng/g are 85.5～91.7% and 74.8～83.1% respectively. The detection limit of the method of determination after trimethylsilylation for DON and NIV are 6ng/g and 8ng/g respectively. The recoveries of DON and NIV added to feed at the range of 20～700ng/g are 81.7～92.6% and 73.8～86.6% respectively, RSD≤4.9%.It shows good precision of the method of determination after fluoroacylation, but the fluoroacylation need heating and spending longer time, the HFB derivatives are more instable than TMS derivatives.The method of determination of DON and NIV by HPLC-MS uses Agilent XDB-C18 as column, methanol-0.1% ammonium acetate solution(20:80,V/V) is used as mobile phase, the toxins ionized by APCI, are determinated by MS using negative ions. Signal 1 is SCAN mode, specific ions are used for qualitative analysis, Signal 2 is SIM mode, selected ions are used for quantitative analysis, and the selective ions for DON and NIV are 295 and 311 respectively.The recoveries of the method for the determination of DON and NIV by HPLC-MS are 91.1～103.6% for DON and 85.6～92.7% for NIV added to the feed at the range of 20～700ng/g . The detection limit is 15ng/g for DON and 18ng/g for NIV, RSD≤5.9%.