HPLC Tandem Mass Spectrometry For High Throughput Detection Of Veterinary Drug Residues

Veterinary drug residue refers to the drug prototype,toxic metabolite or impurities accumulated or stored in the animal cells,tissues or organs after feeding veterinary drugs to the edible animals.These drugs are effective on preventing and curing of animal diseases,as well as improving breeding efficiency.Veterinary drugs which contain quinolones,macrolides,sulfonamides,trimethoprim,?-adrenoceptor agonists,lincosamides or nitroimidazoles,are now widely used in animal husbandry and aquaculture.However,abusing of these drugs could easily lead to severe pollution in aquatic products and edible animals,as they can accumulate in the human body via the food chain,causing allergic reactions and side effects such as drug resistance.Therefore,monitoring multiple veterinary drug residues in the animal products has a positive meaning to food safety issue.In this paper,pork and frozen fillet fish are chosen as the test objects.We study and establish a method of determination of 45 veterinary drugs(quinolones,macrolides,sulfonamides,and ?-adrenoceptor agonists in 4 different categories.Herein,we combine SPE with LC-MS/MS,and study three different solvents used for sample extraction.The optimal condition of 80:20=acetonitrile:water and 0.2% formic acid 80:20 acetonitrile/water solution are used for calculating the recoveries,relative standard deviation,limit of detection,limit of quantitation,and uncertainty of the test methods.At 5~100?g/kg or 0.5~10?g/kg concentration range,excellent linear relations of 45 veterinary drug residues are obtained with the correlation coefficients higher than 0.99.The limit of detection for quinolones,macrolides,and sulfonamides are 0.34~4.59?g/kg with the limit of quantitation to be 1.12~15.31?g/kg.The limit of detection for -adrenoceptor agonists is 0.15~0.48?g/kg with the limit of quantitation to be 0.49~1.49?g/kg.The recovery of these four veterinary drugs is 42.2~130.5%,with the relative standard deviation to be 0.7~41.1%,which meets the requirements of laboratory to become a screening method for veterinary drug residue study.The resource of uncertainty of this method was discussed and evaluated,through it can find out the larger influence of uncertainty factors in the process.Then take action for reduce the impact and improve the credibility of the test results.With the established method for residue detection of 45 kinds veterinary drug in pork and frozen fish fillet,the results of these two samples are all negative.