Study On The Determination Of PFOA By High Performance Liquid Chromatography-Fluorescence Detection With 3-BrAC Pre Column Derivatization

With the wide application of perfluorooctanoic acid（PFOA）,pollution of PFOA has attracted more and more attention.It has toxic effects and has been detected in various environmental media,posing great risks to the ecological environment and human health.The commonly used detection methods of PFOA are expensive and costly,so it is necessary to develop an economical and practical detection method of PFOA.This paper aims to establish a fluorescence detection method for high performance liquid chromatography（HPLC-FLD）and apply it to the determination of PFOA in landfill leachate.In view of the above content,the subject first inspects the derivative effect of two kinds of fluorescently on PFOA,and then determined the suitable fluorescent derivatized agent.The chromatographic conditions and derivation conditions were optimized,and then the HPLC-FLD method was established.The single factor experiment combined with response surface method was used to optimized the solid phase extraction conditions of PFOA in landfill leachate,finally,the content of PFOA in landfill leachate was determined by the established method.The main results obtained were as follows:（1）The characteristic peak of the derivative product of the reaction of 3-bromo acetyl coumarin and PFOA was obvious,and the fluorescence property of the product was stable and the derivative efficiency was high.It was a suitable fluorescent derivative of PFOA.3-bromo acetyl coumarin was suitable to be a fluorescent derivating agent for PFOA;（2）The high performance liquid chromatography-fluorescence detection method for PFOA was established:Zorbax Eclicpse Plus C18 column was selected,the mobile phase was acetonitrile:water（60:40,V/V）,the column temperature was 30℃;10mLPFOA acetonitrile solution was reacted with 1 mL 3-BrAC acetone solution for 150minutes under 70℃,and the derivative concentration was 5mg/mL with 50 mg four Butyl Ammonium Bromide as the catalyst;under the best experimental conditions,through the examination under the test conditions,the PFOA concentration was indirectly measured by determining the fluorescence peak area of the derivatives of PFOA and 3-BrAC and the retention time was 2.78 minutes.The detection limit of the method was 0.007 mg·L^-1 and the quantitative limit was 0.02 mg·L^-1.The application range of PFOA concentration was 0.02¹ mg·L^-1.The derivative solution with PFOA concentration of 0.05 mg/L and 0.5 mg/L was measured respectively,and the recoveries were 86%⁹4%and 92.2%⁹5.8%,and RSD was below 5%.（3）The solid phase extraction conditions of PFOA in landfill leachate were as follows:the activator was 10 mL ammonia methanol（0.01%）,and SPE cartridge was WAX;560 mg of potassium chloride was added to the sample（except untreated leachate）,and the eluent was 6 mL ammonia methanol（0.01%）;the sample volume of landfill leachate effluent after DTRO membrane treatment was 500 mL（the raw leachate was 50 mL）.（4）The high performance liquid chromatography-fluorescence detection method was used to determine PFOA in landfill leachate with accurate results.