Study On The Pretreatment Method Of Drug Residues Detection In Aquatic Products

Food safety has become a global hot issue, which was mainly caused by pesticide residues, veterinary drug residues, heavy metals, feed additives, contaminants and other harmful substances to human health. Due to the frequent occurrence about the quality and safety of aquatic products, antibiotic residues in aquatic products have received much attention. Therefore, it is emergency to develop several kinds of simple operation, convenient and rapid detection inspection and monitoring system for the detection of drug residues in aquatic products. In this thesis, we investigated the pretreatment methods for high sensitivity detection of drug residues in aquatic products by using high-performance liquid chromatography tandem mass spectrometry (HPLC-MS-MS) combined with sample extraction, purification and concentration. The thesis consists of four chapters as followed:In chapter 1, the drug residues and antibiotic of aquatic products were briefly introduced, the technology of pre-treatment samples and analysis and detection methods were described also. Moreover, the purpose and contents of this research had been pointed out.In chapter 2, the sample preparation method of tetracyclines in eel has been developed. In this chapter, we choose four tetracyclines as target and optimize the extracting agent, pH, the adsorption filler of solid phase extraction, the quality of adsorption filler, eluent and synthesis conditions of OTC molecularly imprinted polymer (MIP) for target analytes. In the best condition, the method showed a good linearity in the range of 50～250 μg/L for four targets, the correlation coefficients were between 0.9947 and 0.9994, respectively. The detection limits (LOD) of OTC、 TC、CTC were 10 μg/kg, the LOD of DC were 5 μg/kg.In chapter 3, the sample preparation method of quinolones in eel has been developed. The pre-treatment method of quinolones in eel was mainly researched. We optimized the extraction agent and selected adsorption filler. The ofloxacin molecularly imprinted polymer (OFLMIP) was choose as solid phase extraction column (SPE), the liquid sample was enriched and purified by the SPE. Although the commercial SPE could be used to enrich and purify 11 quinolones, the recovery was low. In this chapter, we synthesized some molecularly imprinted polymer, which filled with solid phase extraction column could purify six kinds of quinolones, and the OFLMIP-SPE could receive high recovery. The LODs of FLU、OFL、ENR、DIF、 OXA and NAA were 2μg/kg,the LODs of NOR, ORB、SPA、SAR and PEF were 5 μg/kg, respectively.In chapter 4, the sample preparation method of nitrofuran metabolites in eel has been developed. In this chapter, the method of rapid derived nitrofuran metabolites was researched. We also optimized the derivative time and derivative temperature. Because of the extraction agent, the target substance was enriched and purified by solid phase extraction column. Then, the sample solution was detected with HPLC-MS-MS. The results showed that the average recoveries of standard addition of three levels were 79.50～108.13%, and the precision of the method was 1.10～6.79%. The LODs of AOZ、SEM、AMOZ and AHD were 0.1 μg/kg,0.5 μg/kg,0.2 μg/kg,0.5 μg/kg, respectively.