The Research Of Separation/enrichment Tetracycline Antibiotics Residues In The Environment By Ionic Liquid Gas-solvent Sublation

Tetracyclines(TCs) antibiotics,especial oxytetracycline(OTC),tetracycline(TC) and chlortetracycline(CTC) have been used extensively due to their broad range of activity against bacteria and their economic advantages.Liquid-liquid extraction and Solid-phase extraction(SPE) have been most commonly used to pre-concentrate for determining TCs.However,the methods are still undesirable for most analyses due to consumption of time and a large amount of volatile,toxic,pollution organic solvents. Additionally,these method can cause secondary pollution and high cost.The aim of the project was to develop a fast and reliable method for the separation/enrichment of TCs antibiotic in environment samples.The method is based on ionic liquid solvent sublation combined with spectrophotometric spectrometry or fluorescence spectrometry or high performance liquid chromatography.It is the first time that ionic liquids and aqueous two phases applied to gas solvent sublation,the method takes a new direction for the flotation process with vast development foreground.The main research contents and conclusion are as follows:(1) Studied on separation/enrichment of TCs antibiotic based on the system of TCs-La(â…¢) by ionic liquid gas solvent sublation,lanthanum nitrate as the trapping agent,the mixture of[Bmim]PF₆ and EA(volume ratio 1/1) as solvent, separated/enriched the TCs residue in the water sample and determinated by spectrophotometric spectrometry,the recoveries ranged from 96.4%to 101.8%,RSD was less than 4.31%.Comparative studied on solvent extraction and gas solvent sublation.(2) Studied on separation/enrichment of TC antibiotic based on the system of TC-Ce(â…¢) by ionic liquid gas solvent sublation,cerium nitrate as the trapping agent, the mixture of[Hmim]PF₆ and EA(volume ratio 1/0.9) as solvent,separated/enriched the TC residue in the chicken,liver and the excrement of the poultry which have been determinated by spectrophotometric spectrometry,the recoveries ranged from 84.6%to 94.0%,RSD was 1.49%to 3.46%.(3) Studied on separation/enrichment of TCs antibiotic based on the system of TCs-Ca(â…¡) by ionic liquid gas solvent sublation,calcium chloride as the trapping agent,the mixture of[Bmim]PF₆ and EA(volume ratio 1/1) as solvent,separated/ enriched the TCs residue in the sample and detected total content by fluorescence spectrometry and moreover researched on the reuse of ionic liquid which can be used repeatedly.(4) Studied on separation/enrichment of TCs antibiotic based on the system of TCs-Fe(â…¢) by ionic liquid gas solvent sublation,ferric chloride as the trapping agent, the mixture of[Omim]PF6 and EA(volume ratio 5/4) as solvent,separated/enriched the TCs residue in the surface water and the sediment of fish pond,the analyte have been detected by fluorescence spectrometry,the recoveries ranged from 94.2%to 100.4%, RSD was less than 3.2%.(5) Studied on separation/enrichment of TCs antibiotic based on the system of TCs-Al(â…¢) by ionic liquid gas solvent sublation,Al(â…¢) ion as the trapping agent,the mixture of[Bmim]PF₆ and EA(volume ratio 1/1) as solvent,separated/enriched the TCs residue in the milk samples detected by high performance liquid chromatography (HPLC).The recoveries of three tetracyclines ranged from 88.5%to 104.0%,the relative standard deviations were between 1.36%and 3.76%.(6) Studied on ionic liquid aqueous two phases gas solvent sublation, [Bmim]BF₄ solution(VN=1) was used as solvent in this experiment with sodium phosphateand as the salt of phase separation,directed trapping and separated/enriched the residue of TCs in pork,detected by HPLC,The recoveries of three tetracyclines ranged from 94.4%to 106.4%,the relative standard deviations were between 1.23%and 4.53%.The results show that ionic liquid gas solvent sublation(ionic liquid aqueous two phases gas solvent sublation) may be thought of a combined method of flotation and solvent extraction(aqueous two phases extraction) with the advantages of both techniques,the method has many merits,such as,non toxic,non pollution,high enrichment factor,high selectivity,negligible emulsion phenomenon,etc.The method is suitable for determining the Tetracyclines residue in environment sample.