Research On The Determination Of Drugs Multi-residue In The Animal-derived Foods

Food safety has always been the hot issues concerned all around the world. The detection method based on liquid chromatography provides technical support to ensure food safety. High performance liquid chromatography(HPLC) method which has superior analytical separation ability has been widely used in the detection of drug residue in the animal-derived foods. Liquid chromatography tandem mass spectrometry both has the excellent separation performance of chromatography and the effective analysis performance of mass spectrometry, which can be used for the simultaneously confirm and accurate quantitative of multi-component analytes in complex sample, it can improve the efficiency of the sample determination significantly. The article includes three partials which were discussed as follows.1 This paper briefly introduces the problem of drug residues in the animal-derived foods. And the research progress of sample preparation at home and abroad and the application of liquid chromatography and its coupled techniques in the detection of drug residues in the animal-derived foods were reviewed.2 A method based on ultra performance liquid chromatography coupled with tandem mass spectrometry(UPLC-MS/MS) was developed for simultaneous determination of 66 kinds of drugs in porcine muscle. The analyte was extracted with acetonitrile-methanol and acetonitrile-water, and was cleaned up by the Agela Cleanert® PEP-2 cartridge. Quantification of the analyte was achieved by UPLC-MS/MS with multiple reaction monitoring(MRM) using external standard method. The results indicated that the detection limits and quantification limits of the method were 0.2 μg/kg~5 μg/kg and 0.5 μg/kg~20 μg/kg. The average recoveries of the drugs ranged from 35%~140% at spiked levels of 2 μg/kg~100 μg/kg with RSD less than 20%.3 A method based on performance liquid chromatography was developed for the determination of 4 kinds of tetracyclines in the muscle, liver, kidney of pig, cow, heep and chicken, etc. The fat sample was dissolved by methylene chloride, then the solution was extracted with Na2EDTA-Mcllvaine buffer solution. The other samples were extracted with Na2EDTA-Mcllvaine buffer solution, and adding sulfuric acid solution and sodium tungstate solution to precipitated protein. All extract was cleaned up by HLB column and LCX column. The results indicated that the average recoveries of the drugs ranged from 64.9%~115.1% at spiked levels of 50 μg/kg ~200 μg/kg in muscle of pig, cow, sheep, chicken, Grass carp, Chinese shrimp and milk, 61.0%~118.5% at spiked levels of 100 μg/kg~600 μg/kg in liver of pig, cow, sheep, chicken and fat of pig and chicken, 62.1%~110.3% at spiked levels of 100 μg/kg~1200 μg/kg in kidney of pig, cow, sheep and chicken, 65.0%~106.0% at spiked levels of 50 μg/kg~400 μg/kg in egg with RSD less than 15%. The detection limits and quantification limits of the method were 20 μg/kg~50 μg/kg and 50 μg/kg~100 μg/kg.