Development Of Certified Reference Materials For Florfenicol And Florfenicol Amine Residues In Prawn

Florfenicol(FF)is a thiamphenicol fluoride developed in the 1980 s.It is a new type of veterinary drug with a broad antibacterial spectrum,low toxic and side effects,and low resistance to drug resistance.The protein synthesis function is widely used in the livestock and poultry industry and aquaculture industry.Florfenicol amine is its main metabolite,and its mark residue.Due to the irregular application of florfenicol in agricultural breeding,it poses a serious threat to human health and public health safety,and its residual problems in animal foods are also increasingly valued.Therefore,florfenicol has been listed as an important monitoring parameter for national and local routine monitoring programs for livestock,poultry and aquatic products.However,after searching the national standard substance resource sharing platform,it was found that florfenicol purity certified reference materials have not been reported,which directly affects the accuracy of the data of the monitoring results.To support government regulation and improve laboratory measurement levels,and to ensure the reliability of florfenicol-related test results,the development of certified reference materials for florfenicol purity is particularly important and urgent.1.Aiming at the research on the certified reference material of florfenicol and florfenicol amine in the prawn,the thesis firstly carried out the certified reference material(CRM)of florfenicol and florfenicol amine in methanol.The development of CRM to establish a complete traceability chain.Two independent approaches involving mass balance method(MB)and the quantitative nuclear magnetic resonance(q NMR)technique were employed to measure the purity of certified reference material(CRM).The homogeneity testing and long-term stability monitoring were examined by high performance liquid chromatography(HPLC).The uncertainty evaluation was sufficiently studied.In this study,chromatographic conditions were optimized for separation of main components and impurities,and several high pure substances were selected and tested as quantitative NMR internal standards.The purity of CRM of florfenicol and florfenicol amine in methaol were accurate,homogenous and stable which satisfy the requirements of CRM..And the purity was 99% and 100 mg/L,respectively.The extended uncertainties are 0.4 and 3 mg/L(k = 2),and they are all successfully declared as CRM(GBW(E)090959 and GBW(E)083588)?2.A method for determining the accuracy of matrix reference materials had established.Using florfenicol-D3 as an internal standard,based on Qu ECHERS method,and liquid-mass spectrometry analysis technology solid-phase pretreatment technology,the establishment of florfenicol residue analysis in prawn meal liquid chromatography-isotopic dilution mass spectrometry was used to accurately measure The residual content of florfenicol drug.The linearity is good within 0.1-50 ?g / kg,The detection limit of the method were 0.1 ?g / kg and the quantification limit of the method were 0.3 ?g / kg.And the recovery rate is between55% and 65%3.Develop certified matrix reference material for florfenicol drug residues in prawn powder.Prawn samples taken for 6 hours in the medicinal bath were prepared through meat extraction,homogenization,irradiation sterilization,packaging,and low-temperature storage to obtain prawn candidates.The established isotope dilution mass spectrometry was used to monitor its uniformity and stability.The results prove that the candidate is stored at-20 ° C,and it is currently stable for 9 months,and short-term transportation can also ensure stability.