| In recent years, with the rapid development of the aquaculture industry, our country has played a important role in aquatic products breeding, consumption and export. There are numerous issues that can’t be ignored have emerged at the same time. One of the most serious is safety problems of illegal drugs exceeded in the aquatic products, It has not only greatly hitted the confidence of the people’s consumption of aquatic products but also restricted the export of aquatic products in our country. Thus, it is urgent to carry out related research of detection method for drug residues in aquatic products.Since the complexity of matrices and diversity of aquaculture medication, the key of residue detection is the selection of the appropriate pre-treatment operation. Magnetic solid phase extraction (MSPE) was used in the field of biochemistry and biomedical engineering. It is convenient to operate and no additional centrifugation or filtration step, so in the field of analytical chemistry gradually as an efficient pre-treatment technology and popularized. In this study, three types of drug residues in aquatic products (Macrolides, Sulfonamides and Quinolones) as the target compound, Homemade magnetic graphene as an adsorbent, the MSPE pre-treatment methods was applied to analysis of residue detection in aquatic products. Considering the different target compounds and the sample matrix, we optimized several critical factor which influence the consequence of pre-treatment and established a MSPE-HPLC-MS/MS detection method for 3 classes drugs residues in aquatic products.1. With the utilization of alkaline solution, we prepared a magnetic graphene nano-materials (G-Fe3O4) which is used to be a magnetic solid phase extraction sorbents. The study characterized its structure by transmission electron microscopy, also, successfully apply it for the pre-treatment of aquatic products. We established a HPLC-MS/MS detection method for Macrolide antibiotics in aquatic products. There was a good linear relationship (R2>0.995) in the range of 1～150 μg/kg; The average recoveries of the method were 87.4%-98.2%. The LOD and LOQ were 0.41～0.52 μg/kg and 1.25～1.65 μg/kg, respectively. The mean values of relative standard deviation of intra- and inter-day were less than 8.5%.2. Thw study established a MSPE-HPLC-MS/MS method by combing magnetic solid phase extraction and HPLC tandem mass spectrometry technology to detect five kinds of Sulfonamides residues of aquatic products. The results showed that a high extraction efficiency was obtained in 10min with extraction solvents of dichloromethane, desorption solvents of methanol/aqueous ammonia(98:2, v:v), reconstitution solvents of 5 mL toluene and 20 mg of magnetic graphene. A good linear relationship (R2>0.992) was obtained in the range of 1-100 μg/kg. The average recoveries of the method were 79.2%-101.3%. The LOD and LOQ for macrolides and lincosamides were in the range of 0.34～-0.49 μg/kg and 1.12～1.47 fig/kg, respectively. The mean values of relative standard deviation of intra- and inter-day were less than 6.2% and 9.2%, respectively. The method we developed was efficient to perform quantitative and qualitative analysis for Sulfonamides residues in aquatic products with a simple and efficient operation.3. The study established a MSPE-HPLC-MS/MS quantitative method for 12 kinds of Quinolones in the aquatic products. We compared 4 kind of pre-treatment about solid phase extraction include magnetic graphene, graphene, C18 cartridge and multi-walled carbon nanotubes, and the results indicated that the magnetic-based solid phase extraction method had a good reproducibility and a high recovery. A good linear relationship (R2=0.991-0.998) was observed in the range of 1-150 μg/kg. The average recoveries of the method were 68.5%-103.4%. The LOD and LOQ for Quinolones were in the range of 0.33-0.95 μg/kg and 1.09～3.14 μg/kg, respectively. The mean values of relative standard deviation of intra- and inter-day were less than 6.2% and 7.8%, respectively. The successful practical application of the proposed method to real samples indicated that the developed method is accurate and effective for detection 12 kinds of Quinolones in the aquatic products. |
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