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Separation And Purification Of Polyphenolic Bioactive Compounds From Rose Using Crosslinked Polymers

Posted on:2012-06-28Degree:MasterType:Thesis
Country:ChinaCandidate:M T M M H M T MaiFull Text:PDF
GTID:2131330335985955Subject:Chemistry
Abstract/Summary:PDF Full Text Request
Polyphenols, rich in plants, are very important plant metabolites, and, has become a hot spot of research and development nowadays because of their various biological characteristics. In order to increase medicinal value of the roses and pomegranate flowers and several new solid-phase adsorption materials were synthesized and packed into the SPE cartridges for separation and purification plant polyphenols.we provide technical support for application of polyphenols separation and enrichment. The main results of the studies are as follows:1. Using 1,2-phenylene diacrylate monomer as functional monomer, and divinylbenzene as cross linking agent, MIP specific for ODB was synthesized; in the same way, using itaconic acid,methacrylic acid,acrylamide and styrene as functional monomers, ethylene glycoldimethacrylate as cross linking agent, crosslinked polymers were synthesized then packed into SPE cartridges. The maximum binding capacity and the best loading conditions were optimised by breakthrough experiment, when the sample loaded at the concentration of 1.0 g ? L -1, in pH = 2 buffer solution on the cartridge, the maximum adsorption capacity of ODB was up to 41.6mg ? g -1; Itaconic acid cross-link polymer after optimized preparation conditions showed surprisingly high binding capacity and their value is 49.5 mg ? g -1.2. After optimization of SPE profile and using Folin -Ciocalteu method, it is determined that the best recovery on the polymer with IA was obtained with loading in 0.1NHCI, washing with water, eluting with methanol: water=95: 5.Polyphenols bound on polymers was up to 55 mg ? g -1,adsorption of polymer obey the normal adsorption patterns,i.e.,Langmuir and Freundlich patterns and obtained good linear fitting;the recoveries of Vc in extract solution were in the range of 98.2% 102.4%. It was found that Folin-Ciocalteu method can be used for the determination of the plant polyphenol contents and correction for underestimate total polyphenol content due to lack of commercial standards and nonelucidate bacause of numerous structures.3. The crosslinking polymers microspheres IA?EGDMA with controllable size were synthesized by suspension polymerization,The effects of various factors,such as disperser PVA weight percentage,agitating rate,the ratio of oil phase to water phase factors,influencing of sphericity and diameter of the microspheres were examined.The chemical structure and morphology of IA?EGDMA were characterized with FT-IR spectrum and SEM respectively. The appropriate conditions: percentage of PVA was 10%, agitating rate was 600 r/min and the ratio of oil to water phase was 1:10. BET analysis showed that surface areas were 214.43m2/g (polymer),144.039 m2/g (resin),129.56 m2/g (microspheres),respectively.4. The first order derivative spectrometry for the determination of was developed using amplitudes at 275nm (peak) and 299nm (valley) with comparable accuracy and precision to the RP-HPLC method and zero order derivative spectrometry,the concentration of nevirapine within 2.5~12.5μg·mL-1 presented a good linear relation (r=0.9997) with the amplitudes and the average recovery was 99.46% (RSD = 1.54%)。Statistical test results showed that there is no significant difference between this method and RP-HPLC method and his method was found to have suppressed the background absorption from the excipients with comparable accuracy and precision, and found to be simple, quick and accurate. It is suitable for quality control of this preparation。...
Keywords/Search Tags:Molecularly imprinted polymers, Crosslinking polymers, Solid-phase extraction, Folin -Ciocalteu method, RP-HPLC, Polyphenols, Microspheres, Nevirapine
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