| Sulfonamide(SAs)is widely used in animal breeding.The drug residues have been discharged into the environment in the form of original drugs and its metabolites.The drug residues could be potentially hazardous to the environment.Based on mixed strong cationic column,the efficient extraction of SAs in different samples has been developed.The new sample pretreatment techniques and HPLC analysis of trace SAs in feeds、animal origin and plasma was established to provide relevant technical support and scientific data for subsequent environmental analysis and safety assessment of SAs.The paper mainly includes the following parts:In chapter 1,literature review.The structure,the physicochemical properties,residual and harmful effects,the pretreatment technique,the mechanism of SAs and its analysis methods were reviewed,and then the aims and research scheme of this study were proposed.In chapter 2,based on polystyrene-sulfonic acid mixed strong cationic column(DBX),the extracting ability of seven SAs(sulfacetamide,sulfapyridine,sulfamerazine,sulfamethoxypyridazine,sulfachloropyridazine,sulfisoxazole and sulfabenzamide)was studied.The effects of various parameters including the matrix of solid phase extraction(SPE)cartridges,extraction solvent,eluent solvent,the amount of solvent on the extracting ability was investigated.The parameters of high efficiency purification technology for seven kinds of SAs in feeds and animal origin was established and used for determining seven kinds of SAs residue in feed and animal tissues.The detection limits in feed and animal tissues were 50.0 μg/L and 40.0～50.0 μg/L,respectively.The average recovery in spiked feed and animal tissues(meat、liver、kidney)were 79.5%～100.9%、85.8%～109.4%、72.5%～105.3%、83.7～108.2%,respectively.The above data show that this method can be applied to detect SAs in feed as well as animal tissues,simplifying the procedure of using two different pretreatment methods in the analysis of SAs in feed and animal tissues.In chapter 3,the rapid pretreatment technology for seven kinds of SAs residues in plasma samples was established.The effect of the parameters including the extraction solvent and the amount of solvent on the extracting ability was investigated.And comparing matrix interference and recovery when the samples treated with DBX column or not,then results indicates that plasma samples without treated with DBX column can achieve the desired effect and realize direct sampling.The detection limits in plasma samples were in the range of 4.0～7.0 μg/L.The recoveries of seven SAs in plasma samples at 50 μg/L,100μg/L and 200μg/L were in the range of 77.0%-105.9%.The above data shows that the method is effective and convenient.In chapter 4,Ethylene glycol dimethacrylate(EDMA)used as crosslinking agent and 2-Acrylamide-2-methylpro panesulfonic acid(AMPS)as functional monomer,a poly(AMP S-co-EDMA)monolithic column was developed and applied for detecting seven kinds of SAs by monolithic column extraction-HPLC.The extraction conditions were optimized,and PMME-HPLC-UV enrichment and analysis methods for seven kinds of SAs was established.Under the optimum conditions,seven kinds of SAs showed a good linear relationship at a linear range of 5～1000μg/L and excellent reproducibility between intra-day and inter-day measure;The detection limits were in the range of 1.00～1.75μg/L.The recoveries of seven kinds of SAs in meat at 10μg/L and 20 μg/L were in the range of 58.3%～90.3%.The above results show that this paper can provide a new technology for high-efficiency extraction and highly sensitive analysis of SAs in environment and food. |
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