Establishment And Application Of Detection Methods Of Five Drug Residues In Aquatic Products

Public announcement No.235of Ministry of Agriculture of the People’s Republic of Chinastipulates the withdrawal period of some veterinary drugs in line with national standards and guidingprinciples, which among the drugs for aquatic products includes: Amoxicillin, ampicillin,Benzylpenicillin,Cloxacillin,Danofloxacin,Deltamethrin,Difloxacin,Enrofloxacin,Erythromycin,Florfenicol,Flumequine,Oxacillin,Oxolinicacid,Oxytetracycline,Tetracycline,Chlortetracycline,Sarafloxacin,Sulfonamides,Thiamphenicol,trimethoprim and more than forty kinds from six categories. Based on thedrugs for aquatic products stipulated in the public announcement No.235, this study displays the liquiddetecting method for31kinds of drugs from five categories (Quinolones, penicillins, tetracyclines,sulfonamides and erythromycin). We also collect the samples of rainbow trout, tilapia, carp, cruciancarp and grass carp which are typical grown in Beijing area. Then we conduct detecting and analyzingon the drugs used on these samples in line with the detecting method in this study.This study used the LC-MS-MS method, the Perch, eel, shrimp, crab and other tissue samples,using internal standard method, the addition of10mL containing0.2%formic acid80:20acetonitrilewater solution extraction,1cc,100mg C18solid phase extraction column purification way establishedmulti residue detection method. The experimental results show that, the method with good linear in theconcentration range of1-500ug/kg, in1ug/kg,5ug/kg,20ug/kg three concentrations, the average rate ofrecovery in the coefficient of variation between58%-95%, less than9.1%, the detection limit is lowerthan0.3ug/kg, the quantitative limit of less than1.0ug/kg, the accuracy and precision of the methodmeets the requirements of drug residue analysis.This study has collected eighty samples of aquatic products in Beijing area and conducted drugdetection with this detecting and analyzing method. The result shows that the drug quantity from aquaticproducts in Beijing area has not exceeded the quantity stipulated by public announcement No.235ofMoA. However, more forbidden drugs from carp and grass carp are detected, especially enrofloxacinwhich is detected from twelve samples,42.16ug/kg at maximum. The drug detected samples come fromChangpin, Pinggu Chaoyang, Fangshan, Haidian, Shunyi as well as Tongzhou, where the detection rateis even among22.2%-40%. There is not any forbidden drugs detected from the samples from Huairou,Miyun and other areas where people grow fishes in natural water.