| T-2 toxin has a strongest acute toxicity,which belongs to the type-A trichothecene mycotoxins.The health of human and animals has been seriously threatened by T-2 toxin,thus how to effectively remove the T-2 toxin in diet has become a currently urgent problem.In this paper,the effect of T-2 toxin removal with benzamide derivatives and ?-CD were studied.The experiments of T-2 toxin removal with benzamide derivatives include five aspects.First,the synthetic method of benzamide derivatives constructed by cross-dehydrogenative-coupling reaction was designed.That is,the benzamide derivatives were synthesized by NMP and benzamide compounds with sp3C-N functionalization reaction.Second,the possible catalysts and oxidants were selected for this reaction.At the same time,the reaction conditions were optimized.Third,the reaction substrates were extended according to the reaction mechanism and reaction pathway of sp3C-N functionalization reaction about benzamide and NMP.Fourth,the effective way of T-2 toxin removal with benzamide derivatives was designed.The reaction solvent for experiment of removal of T-2 toxin was selected.Fifth,the different effects of different temperatures and ultrasound-assisted on T-2 toxin removal with benzamide derivatives were investigated.The different effects of different temperatures,different solvents and ultrasound-assisted on T-2 toxin removal with ?-CD were explored.The results indicate as follows:1.The optimum process of synthesied benzamide derivatives was catalyst of silver nitrate,oxidant of potassium persulfate,temperature of 75 °C,reaction time of 4h,solvent of acetonitrile and water(v/v=1:1).These compounds were the main products of benzamides and NMP reaction according to characterization of the 1HNMR and IR results.The yields of products were between 64 % and 78 %.The method was an effective and green synthesis path to synthesized benzamide derivatives.2.As to the removal of T-2 toxin with benzamide derivatives,under the different temperatures and ultrasound-assisted conditions.Using the mixture of benzoamide derivatives and H2O2(v:v=2:1)to remove T-2 toxin,the molecular ion peak(m/z=490.4192)of T-2 toxin was presented on the products mass spectrum at room temperature.Later,the reaction conditions were changed at 60 °C orultrasound-assisted,there was no molecular ion peak of T-2 toxin on the products mass spectrum.After detoxification the characteristic absorption peaks of the intoxicating group double-bound between C-9,C-10 of T-2 toxin and-CO-NH-group of benzamide derivatives disappeared on the infrared absorption spectrum.It shows that the benzoamide derivatives and H2O2 can not completely remove the T-2 toxin at room temperature,but it is quite possible to remove the T-2 toxin at 60 °C or ultrasound-assisted conditions.The detoxification principle of this experiment is to destroy the intoxicating group double-bound between C-9,C-10 of T-2 toxin to remove T-2 toxin.3.The ?-CD adsorption effect on T-2 toxin was available.There was no high requirement on reaction solvents and reaction conditions.Being convenient,economical,easy to operate and having better removal effect,this detoxication method was acceptable.(1)After reaction in 30 min to 8h at ultrasound-assisted condition in solvents of acetonitrile/ water,ethanol/ water,methanol/ water,DMF/ water,DMSO/ water and ethylene oxide/ water respectively,there was no molecular ion peak of T-2 toxin on the products mass spectrum.(2)After the reaction in temperatures of 25 °C,30 °C,60 °C,90 °C and 100 °C respectively with the reaction solvents and ratio remained unchanged,there was no molecular ion peak of T-2 toxin on the products mass spectrum.In the presence of these six group solvents,no matter at ultrasound,heating,or room temperature,?-CD was able to completely adsorb T-2 toxin and formed host-guest inclusion complex.The removal rates were 100 %.The detoxification principle of this experiment was to form host-guest inclusion complex with ?-CD and T-2 toxin to remove T-2 toxin. |
PDF Full Text Request