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Preparation Of Poly (Butyl Methacrylate-co-ethylene Glycol Dimethacrylate) Monolithic Columns And Its Application In The Determination Of Polycyclic Aromatic Hydrocarbons

Posted on:2012-08-07Degree:MasterType:Thesis
Country:ChinaCandidate:W LiuFull Text:PDF
GTID:2131330332499997Subject:Analytical Chemistry
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Polycyclic aromatic hydrocarbons (PAHs) are organic pollutants existing widely in environment which may lead to carcinogenesis, teratogenesis, and gene mutations. PAHs are considered as prior pollutants in China, the United States, the European Union, and the World Health Organization and International Organizations. At present, the determination methods of PAHs include gas chromatography (GC), liquid chromatography (HPLC), gas chromatography-mass spectrometry (GC-MS), second laser mass spectrometry (L2MS), and enzyme-linked immunosorbent assay (ELISA), etc. In recent years, HPLC is applied to detect toxic and harmful ingredients in the food analysis with high speed and sensitivity.Preconcentration methods are often needed to enhance the sensitivities and decrease the limit of detection because of complex sample matrix and low concentration. Many methods have been used for the sample pretreatment, for example, liquid-liquid extraction (LLE), solid phase extraction (SPE), and solid phase microextraction (SPME), etc. The traditional LLE has the disadvantages of being tedious, time-consuming, and requiring toxic organic solvents which may be harmful to the manipulator's healthy. SPE operation is relative simple and needs less reagent consumption, but multi-step operations are usually necessary. Compared with LLE and SPE, SPME is simple and rapid with low sample consumption and high sensitivities.As a new solid phase microextraction method, polymer monolith microextraction (PMME) technology has been developed in recent years. Monolithic column material is a new material, which has many virtues such as good permeability, small mass transfer resistance, big extraction phase volume, and small dead volume. Because the monolithic column is usually made by situ polymerization method, the monolithic material can be prepared in kinds of upholders. In addition, during the preparation process, it is easy to control the structure, specific surface area, surface properties. These features make monolithic columns have potential applications in the fields of separation and catalysis. Similar to in-tube solid-phase microextraction, PMME technology integrates the advantages of extraction, purification, enrichment, and simple operation. Moreover, PMME decreases the experimental cost because it does not need complex instrument as in in-tube solid-phase microextraction.In the present work, we have prepared poly (butyl methacrylate-co-ethylene glycol dimethacrylate) capillary monolithic column with butyl methacrylate as monomers, ethylene glycol dimethacrylate as cross-linking agent and propanol,1,4-butyl glycol, and water as porogen solvent. PMME has been combined with HPLC method and applied to the analysis of PAHs in meat samples. In order to get higher extraction efficiency, various parameters affecting extraction efficiency have been optimized, such as the extraction flow velocity, extraction volume, and eluent flow velocity. Fine linearity has been observed over the range of 2~10000μg/L for four PAHs, naphthalene, biphenyl, phenanthrene, and anthracene. Regression coefficients of correlation (r) range from 0.9991~0.9999. Under the optimum experimental conditions, the method provides an acceptable linearity, low limits of detection, and good precision. When applied to the determination of the four PAHs in smoked meat samples, recoveries are higher than 80%. The experimental results show that the PMME-HPLC method has the advantages of simple, quick, high sensitivity, and is suitable for conventional analysis of PAHs in smoked meat products.
Keywords/Search Tags:Poly (butyl methacrylate-co-ethylene glycol dimethacrylate) monolith microextraction, polycyclic aromatic hydrocarbons, high performance liquid chromatography, smoked meat products
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