The Preparation Of Matrix Reference Materials For FLU Residue In Eel Muscle

Flumequine is applied in animal production and aquaculture as an antibiotic which brings an extremely significant economic benefits, but the residues of Flumequine drug in animal tissues cause serious harm to human body. Therefore the analysis of Flumequine drug residue has also been duly noted. The research and development of Flumequine physical standard sample of aquatic products towards establishing a kind of analysis methods of Flumequine aquatic veterinary drug residue, determining the experimental accuracy and precision and an important means in the detection of quality control, meanwhile it is an important measure of consumer protection. Therefore, this article separately studied the detection methods of freeze-dried powder and live eel fresh pulp Flumequine and the standard sample preparation methods of Flumequine in eel freeze-dried powder.l.The methods of an ultra-high performance liquid chromatography-tandem mass spectrometry detection of freeze-dried powder and live eel fresh pulp Flumequine veterinary drug residue were established. The samples were hydrolyzed, broken, homogenized in pH=4.5phosphate buffer solution, and extracted by5%methylene chloride+acetonitrile=5+95(v/v), purified by using n-hexane skim off Oasis HLB solid-phase extraction column, and determinated by high performance liquid chromatography-tandem mass spectrometry. The samples were separated by Acquity UPLC BEH C18column, and determinated in the positive ion mode with electrospray ionization tandem mass spectrometry. The validated test was in0.5,1,2u.g/kg3plus standard level, the linear range of methods was0.2-100u.g/kg, the average recovery was86.33%-93.33%, the relative standard deviation was3.41%-10.26%. The minimum determination limit of Flumequine was0.5μg/kg.2.In this experiment, according to the requirements and steps of standard sample of physical production, used the Japanese eel muscle tissue as a carrier, researched and established the prepared methods of freeze-dried powder standard sample of eel Flumequine physical form. Main steps are as follows:the collection and preparation of sample:took out the eels with Flumequine drugs, weighed between200g-300g, removed head, blood, skin, bone and viscera, the high-speed homogenizated into Rouni. Freeze-drying and packaging:After freeze-drying techniques, removed fat by using n-hexane, dried freeze-dried powder by dry boxes made of70"C, vacuumed and sealed bag,5g each bag. Radiation Sterilization:after freeze-dried the samples were in the commission of Compton Radiation Technology Co, Ltd. in Fujian Province, radiation sterilized by Co60-y ray irradiation unit, radiation dose was12KGy, and then stored at-20℃below. Kind of standard samples made the testing of uniformity, stability, and fixing the value. The results showed that:Flumequine positive samples of freeze-dried powder could be uniformly mixed and maked uniformity and stability good; freeze-dried powder valued concentration was11.042μg/kg.