Simultaneous Detection Of 5 Categories 42 Species Of Veterinary Drugs Residues In Aquatic Products And Aquaculture Water

China is a big country of aquaculture,which accounts for about two-thirds of the world's aquaculture productions.However,aquatic products security issues arose frequently in recent years.Veterinary drug residues in aquatic products has become the leading cause of aquatic products security problems,which not only affect the quality of veterinary drug residues in aquatic nutrition itself,but also affect aquaculture water and the related other water.Therefore,the research and development of a kind of rapid detection method of veterinary drugs residues for aquaculture water has great significance.The development of UPLC-MS/MS technology provides the necessary conditions for multi-residues detection;The pretreatment method of Qu ECHERS is simple,fast and efficient,which is widely used in the detection of residues in animal-derived foodstuffs?Solid phase extraction technology is suitable for trace separation,purification and concentration,so,it can be used in pretreatment for aquaculture water's residues detection.This thesis aimed at developing a method for simultaneous detection of 5 species of compounds(including sulfonamides,quinolones,macrolides,lincosamides,nitroimidazoles)the results were summarized as follows:(1)A drug residues detection method of 5 species of 42 kinds of compounds was established.The parent ions,collision energy,and cluster voltage of 42 kinds of compounds and 6 kinds of internal standard were optimized;A reversed phase Waters BEH C18 analytical column was selected for chromatographic separation of the drugs in sample,elution solvents used acetonitrile and ultrapure water which added 0.1% formic acid with gradient elution.(2)The pretreatment method of Qu ECHERS for 42 kinds of veterinary drugs was developed.The optimal method of pretreatment method were achieved with 5% acetic acid in acetonitrile as extraction solvent,1 g Na Cl and 4 g Na2SO4 as salting-out agent and absorbent agent,150 mg C18 and 50 mg PSA as the purifying filler.(3)Using solid phase extraction,an effective pretreatment method of 42 kinds of veterinary drugs was established.The solid phase extraction column,p H of the solution and eluent were optimized through the experiment.The sample was was adjusted p H to 5 with formic acid,and then purified by an Oasis HLB extraction column,eluted by containing 5 mmol/L ammonium acetate 0.1%(m/v)aqueous formic acid,and finally eluted with methanol.(4)Methodology validation of the detection and pretreatment method were done based on the aquatic products and aquaculture waters.Whether in aquatic products or aquaculture waters,the matrix compounds were weakened.The specificity and the limit of detection and quantitation in two substrates can meet the needs of real samples.Aquatic products:The recovery of 42 kinds of veterinary drugs was 55.32%-128.36%,RSD was 0.52-20.01%,LOD was from 0.01 to 0.15 ?g/kg,LOQ was from 0.02 to 0.45 ?g/kg;Aquaculture waters:The recovery of 42 kinds of veterinary drugs was between 66.02% and 131.06%,RSD was between 0.80% and 28.86%,LOD and LOQ was 0.01-0.17?g/kg and 0.03-0.45 ?g/kg.(5)The results showed that enrofloxacin in aquatic products was the highest detection rate of veterinary drug,veterinary remaining species were also detected,but the detection of veterinary drug levels were well below the maximum residue limits of the provisions of(MRLs)value;as a forbidden veterinary drugs,ciprofloxac was also found.The detection rate of veterinary drugs in aquatic products was lower than in aquaculture water,but the contents were in the low ppb range.