Study Of Novel Rapid Synergistic Cloud Point Extraction For Quantitative Analysis Of Alkylphenols And Bisphenol In Water Samples

Phenolic compounds are one of the most important pollutants in the environment,which are widely used and toxic,and can pose a serious threat to organisms.Among them,bisphenols and alkylphenols have potential adverse effects on the human body even at trace levels,especially because of their environmental endocrine disruption properties,which have attracted more and more attention.Therefore,it is necessary to establish an environmentally friendly,rapid and accurate method to monitor the content of phenolic compounds.However,the content of bisphenols and alkylphenols in the environment is low,and the environmental matrix is complex,which has become the bottleneck of accurate qualitative and quantitative analysis.The key point to solve this problem is to purify,enrich and separate the samples by appropriate sample preparation techniques.In this paper,a new rapid synergistic cloud point extraction?RS-CPE?technology with simple operation,green environmental protection and high enrichment multiple,and great development prospects is used as a sample pretreatment technology.It is combined with high performance liquid chromatograph to establish the relevant detection method,and the extraction mechanism is preliminarily discussed.The specific research contents and results are as follows:In the first chapter,the current situation and harm of phenolic compounds in the environment are summarized,as well as the application and development of various pretreatment technologies in the enrichment and separation of phenolic compounds.And they are mainly discussed that the improvement methods and research progress of cloud point extraction.Finally,the research background and content of this paper are described.In the second chapter,an acetonitrile RS-CPE method was established for determination of six bisphenols by HPLC with fluorescence detection.In this experiment,the non-ionic surfactant?Genapol x-080?was selected as the extractant,and acetonitrile was used as the synergistic reagent with Na₂SO₄ to reduce the cloud point temperature of the extractant to room temperature.The whole experimental process was rapid and simple.The affecting factors such as the concentration of Genapol x-080 and Na₂SO₄,the volume of acetonitrile and the pH of solution were studied.Under the optimized experimental conditions,the correlation coefficient?r?was greater than0.9982,the limit of detections?LOD?were 0.024-0.032?g/L,the relative standard deviation?RSD?intra-day and inter-day were less than 5.31%,and the extraction rates were more than 89.15%.In the third chapter,a RS-CPE method with environmentally friendly ionic liquid 1-hexanol-3-butylimidazole bis?three fluoromethylsulfonyl?imine as a synergistic inducer was established for the determination of six bisphenols by HPLC.The functional ionic liquid with good polarity was selected as synergistic inducer.Because it contained a hydroxyl group,it could form a stronger interaction with bisphenols and obtain a high extraction rate,which solved the low extraction efficiency of traditional CPE for phenols.At the same time,the process of RS-CPE could be completed at room temperature,making the whole experimental process simpler,time-saving and labor-saving.The type and concentration of ionic liquid,surfactant,inorganic salts,the pH of the solution and the centrifugal speed were studied.Under the optimal conditions,the five bisphenols and BPPH value were in the range of0.125-65.0?g/L and 0.250-65.0?g/L?r>0.9974?,the limit of detections were 0.028-0.045?g/L,RSD of intra-day and inter-day<4.76%,and extraction rates were 87.61-97.38%.The method has been applied to the determination of six bisphenols in environmental water samples with a recovery of 90.7-107%.The results showed that this method had the advantages of simple operation,friendly environment and good extraction efficiency,and it was suitable for the determination of this kind of target in actual water samples.In the fourth chapter,in order to verify the universality of the above method,the method established in the third chapter was applied to the determination of nine alkylphenols.By further comparing the extraction effects of seven different ionic liquids,a low-viscosity,easy-to-handle,economical,environmentally friendly and the best extraction effect on nine alkylphenols ionic liquid 1-ethyl-3-methylimidazole bis?fluorosulfonyl?imide salt was selected as a synergistic inducer,while optimizing other factors affecting extraction efficiency.Under the optimal experimental conditions,the nine target substances have good linearity and high response?r?0.9990?in the concentration range,and the precision is good?intra-day and inter-day of RSD is less than 5.59%,n=6?.The established method is applied to the determination of these substances in actual water samples,and the recovery rate is between92.1-108%.The experimental results showed that the method had been successfully applied to the separation,enrichment and determination of nine alkylphenols with satisfactory results.