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The Research And Application Of New Solid Phase Microextraction Technique In The Analysis Of Environmental Samples

Posted on:2017-01-07Degree:MasterType:Thesis
Country:ChinaCandidate:N N GaoFull Text:PDF
GTID:2334330482495546Subject:Drug Analysis
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With the development of science and technology, scientists make their efforts to find a quicker, more accurate, more sensitive, less expansive, and greener method to analysis the pollutants in the environment. Due to the low concentration of organic pollutants, complex matrix, and distractors in the environmental samples, how to make a quick and simple pretreatment for the samples has been a great challenge all the time. Among all the separation and concentration techniques, the magnetic solid-phase extraction(MSPE) has gained more attention due to its simple operation and high extraction efficiency. In this paper, we carried out the following work by combing the adsorption performance of natural mineral loaded magnetic nanoparticles for drugs:Firstly, we briefly introduced the magnetic solid-phase extraction methods, summarized the structure and property of nanometer materials and the application of functionalized magnetic nanoparticles in MSPE.Secondly, we developed a two-step method to extract and concentrate alfuzosin hydrochloride(ALF) by integrating the micelle cloud point extraction(MM-CPE) and magnetic dispersive ?-solid phase extraction(MD-?-SPE). The mixed micelle anionic surfactant, sodium dodecyl sulfate and non-ionic polyoxyethylene nonylphenylether were used as the extraction solvent in MM-CPE, and the diatomite bonding Fe3O4 magnetic nanoparticles(DMNPs) were used as the adsorbent in MD-?-SPE, respectively. In this method, ALF was extracted into the surfactant-rich phase, then gathered by the magnetic materials, and separated from the aqueous phase by an external magnetic field at last. A linear relationship in the range of 5-300 ng/m L and a limit of detection up to 0.16 ng/m L were obtained at the optimal condition. This method has been successfully applied in the detection of drugs, urine, and plasma.Thirdly, we have successfully fabricated four kinds of natural magnetic adsorption, bentonite, attapulgite clay, kaolin, diatomite loading Fe3O4 magnetic nanoparticles(BMNPs, AMNPs, KMNPs, DMNPs) and studied its adsorption and desorption capacity for the 12 kinds of quinolones, respectively. The experimental results showed that the highest extraction rate of each magnetic adsorbent was: 99.98%, 99.99%, 36.78%, 23.65%, respectively. The extraction capacity of BMNPs was as high as that of AMNPs, and the extraction ability of KMNPs, DMNPs were relatively low. Besides, a fast, efficient and sensitive method was developed to determinate the six kinds of quinolone antibiotics(ciprofloxacin, difloxacin, enrofloxacin, norfloxacin, sarafloxacin and lomefloxacin) in milk by using the magnetic bentonite as the extraction agent and followed by the high performance liquid chromatography and the fluorimetric detection. A linear relationship for the six quinolones in the range of 0.2-200 ng/m L and a correlation coefficient of the calibration curves ranged from 0.9994 to 0.9999 were obtained at the optimal condition. The limit of the method was 0.1 ng/m L and the recoveries of the two milk samples varied from 80.4% to 92.7% and 81.3% to 93.5%, respectively.In the end, a novel and simple method to absorb the Pazufloxacin mesylate(PZFX) in urine and blood samples was developed and used in fluorimetric detection. Besides, a kind of AMNPs nanocomposites was fabricated and used as the adsorbent in the the MSPE. A linear relationship in the range of 2-36 ng/m L and a correlation coefficient of 0.9998 were obtained at the optimal condition. The limit of the method was measured to be 0.1 ng/m L. The results showed that the proposed method can detect the PZFX in urine and plasma rapidly, reliably, and efficiently.
Keywords/Search Tags:Magnetic solid-phase extraction, Natural mineral clay, Quinolone, Mixed micelle cloud point extraction, Magnetic dispersive ?-solid phase extraction, Alfuzosin
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