Determination Of Sulfonamides Residual In Aquatic Products Of Ningbo By UPLC-MS/MS

With the development of agriculture, for the disease control and prevention and the illegal growthpromoting, kinds of sulfonamides are widely used in aquatic products breeding. The unreasonable using ofsulfonamides, will lead to the excess residue in fish tissue, and cause harm to human body allergic reactionsto drugs, inhibit the hematopoietic system, urinary system and central nervous reaction, etc through thefood chain. There are many different kinds of sulfonamides, and the range of traditional detecting method issmall, with low sensitivity, corroborate difficulties. So we need a simple processing, extraction efficiencyand wide adaptation detecting method for sulfonamides. The article is mainly for the research of the levelof sulfonamides residues in the breeding aquatic products with ultra performance liquid chromatography-tandem mass spectrometry. Adopt the method of reverse study, optimized test conditions from the massspectrum attune, gradient elution, evaporate concentration, solid phase extraction, extraction reagent,processing method, etc to achieve an ideal results. Experimental results show that leaching sample with themethanol-acetonitrile (2+1) secondary, remove fat, analyzing after SPE column purification, use theUltiMate3000ultra high performance liquid chromatography (HPLC) and TSQ Quantum Acess MAXtandem mass spectrometer coupled for qualitative and quantitative research,24kinds of sulfonamidesresidues can complete separation in a short time. The LOD is0.3μg/kg, the LOQ is1.0μg/kg, The curveregression coefficient of24kinds of sulfonamides is≥0.998, in the range of4～40ng/mL. In10,50,200,μg/kg, the scope of recovery is over85%, the relative standard deviation is≤5%. This method’spretreatment method is easy and simple, with high efficiency, wide linear range low detection limit, highsensitivity and detection of objects is wide.Sampled traditional farmed fish, products of aquaculture products, imported varieties breeding aquaticproducts and other kinds of samples, a total of163batches from34aquaculture farms in Ningbo. Use themethod in this paper to analyze the163batches of samples, fifteen samples were detected positive quantityof sulfonamides residual with different types and levels, but no more than the limit in "NY5070-5070Pollution-free food Fish drug residues in aquatic products limited".