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Research On The Sample Preparation Techniques Of Polycyclicaromatic Hydrocarbons In Different Matrices

Posted on:2015-03-13Degree:MasterType:Thesis
Country:ChinaCandidate:W L HeFull Text:PDF
GTID:2181330431978019Subject:Pharmaceutical engineering
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Polycyclic Aromatic Hydrocarbons are contaminant widespread in the environment, which mainly from the process of human activity and energy use. The study show it is carcinogenic, teratogenic and mutagenic, so it may cause some harm to the human health and the environment. It has been included in the list of priority pollutants for it attracted more attetions. Therefore, it is quite important to build some accurate and convenient methods for the determination of PAHs. we have studied several methods based on high performance liquid chromatography to determin benzo (a) pyrene, Benzo (a) anthracene, benzo [b] fluoranthene,, The main research contents are as follows.Parti Vortex-Shaking-Assisted and Supramolecular Solvent-Based Microextraction Followed by HPLC-FLD Determination of Benzo(a)pyrene in Water SamplesA supramolecular solvent made up of nonanoic acid aggregates is proposed for the extraction and reconcentrating of benzo(a)pyrene in water sample. The procedure involved the extraction of water sample (9mL) with the supramolecular solvent made up of250μL nonanoic acid and1mL tetrahydrofuran. Vortex-shaking was applied to enhance the extraction efficiency. Parameters affecting the extraction of target analytes including the selection of the alkylcarboxylic acid, the percentage of tetrahydrofuran, the amount of decanoic acid, temperature, extraction time and centrifuging time were investigated. Under the optimum conditions, the linear range of benzo(a)pyrene was10-800ng·mL-1, the correlation coefficient of the calibration curves was0.9999, the relative standard deviations (RSD, n=5) were1.44-4.79%and the limits of detection (LOD) was4.1ng·mL-1in water samples. The results indicated that the method is simple and rapid,while delivering accurate and precise results and can be used for the determination of benzo(a)pyrene in water samples.Part2Determination of polycyclic aromatic hydrocarbons in three junk food Using Microwave-vortex-assisted liquid-liquid microextraction combined with HPLCIn this study, microwave-vortex-assisted liquid-liquid microextraction (MAE-VA-LLME) was developed as a simple, rapid, and efficient method for extraction of three polycyclic aromatic hydrocarbons (PAHs) in three junk food followed by high performance liquid chromatographic-fluorescence detector (HPLC-FLD) analysis. For this purpose, PAHs were extracted from the food matrices samples using a MAE method into KOH (2M) and ethanol (6:4, v/v). Subsequently, a VA-LLME procedure was applied on the MAE extracts and the analytes were determind by HPLC-FLD. Under optimal conditions, linearity of the method was in the range of0.25-50μg kg-1food (dry weight). The relative standard deviations in real samples varied from2.17%-4.21%(n=5). The proposed method was successfully applied to analyze the target PAHs in three soil food samples, and satisfactory results were obtained.Part3Votext-assisted liquid-phase microextraction based on a nanostructured supramolecular solvent in aqueous samples.A new simple and sensitive method has been developed for the determination of trace levels of polycyclic aromatic hydrocarbons (PAHs) inl aqueous samples.It is based on the use of nanostructured supramolecular made up of Ionic liquids1-Butyl-3-methylimidazolium tetrafluoroborate ([BMIM]BF4) and n-Octanol. This method breaks the classic supramolecular solvent composition and use votext accelerated mass transfer of the target analytes into the nanostructured solvent from the aqueous sample, thus reducingextraction time. Factors affecting the extraction were optimized, Under the optimized conditions, The linearity correlation coefficient of the metho were0.99-1over the range0.5-100ng mL-1.The detection limits of the method were0.046-0.092ng mL-1. The relative standard deviations from1.79-4.51%. This method was successfully used for analysis of polycyclic aromatic hydrocarbons in wine and beverages, with good recovery of spiked polycyclic aromatic hydrocarbons over92%.
Keywords/Search Tags:Polycyclic aromatic hydrocarbons (PAHs), high performance liquidchromatograph, Microwave-vortex-assisted liquid-liquid microextraction, Supramolecular solvent, Junk food
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