| This study used the QuEChERS pretreatment method,combined with High-performance liquid chromatography tandem mass spectrometry,a method was developed for the determination of 54 target compounds in aquatic products,including Sulfonamides,Quinolones,Macrolides,Nitroimidazoles,Tetracyclines,Receptor agonists,Chloramphenicol,etc.,the research contents and results were as follows:1.With the development of economy and society and the improvement of people’s living standard,the problem of veterinary drug residue has become the focus of attention.At present,blind drugs aggravate the residues of veterinary drugs in aquatic products,which make the drugs and their metabolites remain in food of animal origin,thus posing a potential threat to human health.In order to protect public health and safety,a reliable analytical method is urgently needed for the determination of veterinary drug residues in edible tissue samples(such as fish,meat and poultry).Because of the great differences in the physical and chemical properties of various veterinary drugs,it is difficult to determine many kinds of veterinary drug residues at the same time.Therefore,it is urgent to develop a sensitive,reliable and simultaneous detection technique for multi-veterinary drug residues.2.In this study,pseudoscoaena crocea was extracted with acetonitrile containing 0.1%formic acid as solvent,0.2% formic acid water-0.2% formic acid acetonitrile as mobile phase,and anhydrous sodium sulfate as dehydrating agent,the mixture of 150 MG octadecyl Bonded Silica Gel(C18)and 50 mg ethylenediamine-n-propyl Silane(PSA)was selected as the purifying agent.The complex solution was acetonitrile-0.1% formic acid water(10:90,V / V),quantitative analysis identified 54 of the target compounds.3.In this experiment,the large yellow Croaker was taken as the research object,and the methodology was validated according to the above methods.The results showed that all the 54 target compounds showed good linear relationship in a certain range,the correlation Coefficient was more than 0.9940,the average recovery was 66.6%-116.4%,the relative standard deviation was less than 7%,the quantitative limit is 0.5-15.0 g/kg,and the detection limit is 0.1-5.0 g/kg.Accuracy and sensitivity meet the experimental requirements,and can be used for the detection of multi-veterinary drug residues in aquatic products.The method was applied to the determination of 50 batches of large yellow Croaker,in which the residues of Ofloxacin and Enrofloxacin were detected in 2batches.Compared with the results of the existing standard method GB/T 20366-2006,the difference of the determination values was not significant,and the RSD was less than3%,it shows that the method is accurate and feasible.4.Taking River Shrimp as the research object,the method was further validated.The results showed that the average recovery of 54 target compounds was between 64%and 114%,and the correlation coefficient was above 0.9900,the range of quantitative limit is 1.0-15.0 g / kg,the precision and accuracy of the method are good,and it meets the requirements of aquatic products detection.According to the established method,more than 100 samples of 9 kinds of aquatic products were detected in 6 kinds of veterinary drugs.Compared with the existing standard method,the result difference was not big,RSD was less than 9%,which showed that the method had good accuracy and repeatability. |
