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The Studies On Molecularly Imprinted Solid Phase Extraction And Solid Phase Microextration Of Dibutyl Phthalate

Posted on:2011-06-22Degree:MasterType:Thesis
Country:ChinaCandidate:R H LvFull Text:PDF
GTID:2121330332465342Subject:Analytical Chemistry
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Molecular imprinting polymers (MIPs) were prepared by bulk and suspension synthesis. The conditions of experiment were optimized and binding characteristics were evaluated. The structure of the MIP was confirmed by Fourier transform infrared spectrometry and thermal stability was investigated by Thermal Analyzer. Scanning electron microscopy was employed to monitor morphology of the MIPs. MIPs were used as sorbent of solid phase extraction (MI-SPE) and the coating material of solid phase microextration (MI-SPME), then they were applied to analysis real samples. The main research results are as below:1. Molecularly imprinted polymers of dibutyl phthalate (DBP) were prepared by bulk polymerization. The optimum condition was obtained. The ratio of template molecule (DBP) and functional monomer (methacrylic acid) to crosslinking agent (ethylene dimethacrylate) is 1:6:30. The molecular recognition and binding characteristics of the polymer were studied. The polymers were loaded into the solid phase extraction cartridge. With optimum washing and elution solvent, MI-SPE showed high affinity and specificity to DBP compared with non-molecularly imprinted solid phase extraction (NI-SPE) for water samples, the absorption amount of DBP were 426.07μg g-1 and 219.81μg g-1. The method of the determination of DBP in water samples has been developed using MI-SPE. The linear ranges of the method was 0.005-0.1 mg mL-1 and the limits of detection was 0.013 mg mL-1. The recovery of matrix spiked samples were 97.9%,106.4 %,91.5 and 99.8%, and the relative standard deviation (RSD) of were 16.21%,7.83%,5.34% and 4.29% at levels of 0.5μg mL?1,1μg mL?1,4μg mL?1和8μg mL?1, respectively. Finally, the MI-SPE cartridge were used to detect DBP in the soybesn milk, the detected amounts of diethyl phthalate (DEP), DBP and dioctyl phthalate (DNOP) were 7.6μg L-1, 8.8μg L-1 and 9.6μg L-1。2. The imprinted molecular microspheres (MIMs) of DBP was prepared by suspension polymerization, and then the MIMs were used as absorbent to analysis real water samples. The selective experiment results showed that the absorbed amounts of DBP were 736.85μg g-1 and 401.58μg g-1 by MIM and non-imprinted molecular microspheres (NIMs). The recovery of matrix spiked samples were 102.5 %,104.5 % and 99.5 %, and the RSD were 1.5 %,5.7 % and 2.1% at levels of 0.25μg mL-1,1.25μg mL?1 and 2.5μg mL-1, respectively. The result indicated that the method have higher recoveris, good reproduction and lower detections in detection of real sample. And the MIM-SPE cartridge were used to detect in the rever sample, the detected amount of DEP, DBP, diamyl phthalate (DAP) and DNOP were 7.6μg L-1, 8.8μg L-1 and 9.6μg L-1, and also detected DEP and DBP in the reservoir were 9.5μg L-1和13.3μg L-1。3. A novel MI-SPME fiber was prepared with DBP as the template molecule. The SPME device was modified from commercial syringe and the MIP fiber which was prepared by polymerizing in the inner of the glass capillary. The fiber was flexibility, and much cheaper than the commercial SPME fiber. It could couple with gas chromatography easily. The MIP fiber had higher selectivity absorption of 154.72 ng than NI-MIP fiber of 28.03 ng. The averge recoveries of matrix spiked samples were 99.91 %, and the RSD of were 2.2 %,7.8 % and 5.3% at levels of 0.5μg mL-1, 2.0μg mL?1 and 5.3μg mL-1, respectively. And the MI-SPME were used to detect in the bottle water sample, the detedted amount of DMP, DEP, DBP and DAP were 0.10,0.22,0.23 and 0.07μg L-1, and also detected DMP, DEP, DBP and DNOP in the reservoir is 0.10,0.25,0.53 and 0.27μg L-1。...
Keywords/Search Tags:Molecularly imprinted polymer, Solid phase extration, Solid phase microextration, Dibutyl phthalate
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