The Application Research On The Technology Of Q-TOF In The Screening Of Drug Residues In Animal Products

The ultra performance liquid chromatography-quadrupole time-of-flight massspectrometry (UPLC-Q-TOF) is a new analytical instrument which combines goodseparation ability of chromatography with high resolution of mass spectrometry. Inrecent years， because of its high resolution in wide quality coverage， obtaining theexact distribution of isotopic peak， the capability to measure exact masses of parention and daughter ion，Q-TOF is widely used in analysis of food safety，bioanalysis，pharmaceutical analysis， environmental monitoring and metabonomics. Withfrequent incidents of food safety， food safety issues have attracted considerablepublic attention. More and more testing organization and research department applyQ-TOF to the screening. The main contents of this paper were described as follows:1. The actuality of veterinary drug residue in food animals and food safety werebriefly reviewed，on the other hand，multiclass-multiresidue methods for veterinarydrugs and the usage of UPLC-Q-TOF in food safety were summarized.2. A method based on ultra performance liquid chromatography-quadrupoletime-of-flight mass spectrometry (UPLC-Q-TOF) has been developed for quantitativeanalysis of74kinds of veterinary drug in chicken. The chicken was extracted withacetonoitrile and5%trichloroacetic， purified with a500mg Waters Oasis HLB SPEcartridge. The linearity of respond ranged from10μg/L to1.5×104μg/L and thecorrelation coefficient was greater than0.98. The average recoveries ranged from30%to130%of74kinds of veterinary drug in chicken at three different levels. The limitsof detection were ranged from0.5μg/kg to10μg/kg.3. A new screening method for6sedatives in beef by ultra performance liquidchromatography-quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF) hasbeen developed. The sedatives were extracted by acetonoitrile for twice and purifiedby NH2cartridge. The accurate mass was obtained under different levels and theaccuracy error was lower than7×10-6. The correlations of6sedatives were greaterthan0.98between2ng/mL and50ng/mL. The limits of detection of6sedatives werefrom0.5μg/kg to1μg/kg. The average recoveries ranged from60%to90%of the fortified6sedatives in beef at2μg/kg~10μg/kg levels. The results showed that themethod was highly sensitive and selective for screening of6sedatives in beef.4. The method of application of screening software was briefly introduced in thisthesis and the developed methods were already used in the screening for veterinarydrugs residue in commercially available food animals. It was indicated that somekinds of antibiotic were spiked in food animals， however， after quantitativeresearch， lots of them were reasonable use and a small number were illegal use.