| Tetracycline antibiotics(TCs) include primarily oxytetracycline(OTC), chlortetracycline(CTC) and tetracycline(TC),other types include semi-synthetic methylene oxytetracycline,doxycycline and tetracycline dimethylamino,which are widely used in disease prevention,control and treatment of livestock and poultry,aquatic animal and plant.The residual substances of TCs which enter into the environment via various channels are toxic and difficult to biodegradation.TCs in the soil,plants,food and animal waste would eventually enter the natural water body,and that,the residue of TCs would be transfered to flora,fauna and human body from water.This is a serious threat for the natural ecological balance system and human health.The analysis methods of TCs residue have HPLC,HPLC-MS,ELISA and so on.These studies focus on the residual analysis in food and soil and very few related to the separation and enrichment of TCs in water.In this thesis,we would first set up a green and new integrated technique,which combines separation and collection with analysis.Furthermore,the behaviour of separation and preconcentration of the technology to the TCs residues in water was investigated.The aim of the research is to build a foundation of theory and practice for controlling the pollution of TCs residues,the main research contents are as follows:(1) The new separation and preconcentration technology of hydrophilic organic solvent floatation(HOSF) has been set up on the basis of traditional organic-solvent extraction,which coupled the advantage of hydrophilic organic solvent eatraction and solvent floatation.The water-soluble polymer,small molecule organic solvent and ionic liquid used in aqueous two-phase extraction are koown as the three main types of green solvents,the technology of solvent floatation is a efficient method of separation and enrichment,the new system is built by a combination of both.The basic work principle of the technology was illustrated,test model was created,test equipment was designed and producted.Moreover,the hydrophilic organic solvent,trapping agent and phase-separating salt were screened and modified,effectiveness of the methodology were studied.(2) Studied the coordination chemical reaction of Fe(Ⅲ),Co(Ⅱ),Ni(Ⅱ),Cu(Ⅱ),Mg(Ⅱ),Ca(Ⅱ),Al(Ⅲ) with TC,OTC,CTC and the ternary association of Co(Ⅱ)-OTC,Ni-CTC with DAN,we found that the formation of new compounds improved significantly the hydrophilic properties of TCs,the TCs are transformed into hydrophobe from hydrophilic matter.The achievement improved the sensitivity and efficiency of separation and preconcentration of trace TCs in water by HOSE(3) The behavior of separation and preconcentration on the trace OTC in environmental water samples was studied by HOSE Calcium chloride as the trapping agent,the mixture of n-propanol and n-butyl alcohol(volume ratio 4/1) as solvent,the OTC residue in aquaculture wastewater has been separated,preconcentraed and determinated.The potential effects of test parameters on separation and preconcentration were investigated, concentration and the absorbance measured in the range of two orders of magnitude showed good linearity.The detection limit is 2.43×10-7 mol/L,recovery is more than 97%:Cobalt(Ⅱ) and DNA as the two-way trapping agent,tetrahydrofuran as solvent,the OTC residue in pharmaceutical wastewater has been separated,preconcentraed and determinated.The potential effects of test parameters on separation and preconcentration were investigated,concentration and the absorbance measured in the range of there orders of magnitude showed good linearity.The detection limit is 3.82×10-9 mol/L,recovery is more than 99%.(4) The behavior of separation and preconcentration on the trace CTC in environmental water samples was studied by HOSE Iron nitrate as the trapping agent,the mixture of tetrahydrofuran and ethanol(volume ratio 4/1) as solvent,the CTC residue in Ruhe water and Zhanhe water has been separated,preconcentraed and determinated.The potential effects of test parameters on separation and preconcentration were investigated, concentration and the absorbance measured in the range of two orders of magnitude showed good linearity.The detection limit is 3.39×10-7 mol/L,recovery is more than 96%;Nickel(Ⅱ) and DNA as the two-way trapping agent,tetrahydrofuran as solvent,the CTC residue in urine has been separated,preconcentraed and determinated.The potential effects of test parameters on separation and preconcentration were investigated, concentration and the absorbance measured in the range of there orders of magnitude showed good linearity.The detection limit is 1.8×10-9 mol/L,recovery is more than 99%.(5) The behavior of separation and preconcentration on the trace TC in environmental water samples was studied by HOSE Copper sulfate as the trapping agent,n-propanol as solvent,the TC residue in medical wastewater has been separated,preconcentraed and determinated.The potential effects of test parameters on separation and preconcentration were investigated, concentration and the absorbance measured in the range of two orders of magnitude showed good linearity.The detection limit is 9.0×10-7 mol/L,recovery is more than 97%;Aluminium(Ⅲ) chloride as trapping agent,n-propanol as solvent,the TC residue in groundwater has been separated,preconcentraed and determinated.The potential effects of test parameters on separation and preconcentration were investigated, concentration and the absorbance measured in the range of two orders of magnitude showed good linearity.The recovery is more than 99%; Magnesium(Ⅲ) chloride as trapping agent,tetrahydrofuran as solvent,the TCs residue in lake water has been separated,preconcentraed and determinated.The potential effects of test parameters on separation and preconcentration were investigated,concentration and the absorbance measured in the range of two orders of magnitude showed good linearity. The recovery is more than 96%.The results of the study showed that the technique of hydrophilic organic-solvent floatation is an efficient method of separation, preconcentration and detection of TCs residues in water,the application process does not produce secondary pollution.
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