XIA Ran , SUN Li-Ping , QU Gui-Rong
2016, 33(3).
Abstract:Non-costly and readily available inosine was transformed into 2′,3′,5′-tri-O-acetyl-6-chloropurineside via acetylation of sugar and chlorination of C6 carbonyl group. Then the nitro group was introduced into C2 of 2′,3′,5′-tri-O-acetyl-6-chloropurineside in CH2Cl2 with n-Bu4NNO3 and trifluoroacetic anhydride. The final product 2,6-dichloropurine riboside was synthesized in 63% total yield in HCl/EtOH solution which de-protected the acetyl groups and chlorinating the nitro group in one pot and two steps. The effects of nitro precursor, chloro precursor and reaction scales on the yields were investigated. The yield was maintained even on the 200 g scale.
ZHOU Juying , ZHANG Lingyu , LI Pengfei , HUANG Qin
2016, 33(3).
Abstract:槲皮素;马来松香丙烯酸乙二醇酯;分子印迹聚合物;吸附性能
2016, 33(3).
Abstract:To improve and optimize the synthetic process of 3-amino-2(1H)-quinolone ring, 3-amino-7,8-dimethoxyl-2(1H)-quinolone (VII) was synthesized by the reduction of 3-nitro-7,8-dimethoxyl-2(1H)-quinolone (IV), which was prepared by the cyclization of 2-amino-3,4-dimethoxylbenzaldehyde (V) with methyl nitroacetate. The compound V was successively prepared from vanillin via actylation, nitrolation, methylation and reduction. The results showed that preferred synthetic conditions were as following: the piperidine catalyzed the cyclization reaction in the mixed solvent of toluene and cyclohexane in volume ratio 7: 3, the 5% Pd/C and ammonium formate were used as the reduced system to reduce the compound VI. The synthetic yield of the 3-amino-7,8-dimethoxyl-2(1H)-quinolone could reach higher than 70%, calculated from the O-aminobenzaldehyde V.
2016, 33(3).
Abstract:In order to improve the prunin yield, simplify the process of separation and purification and obtain the high purity production, the conversion of naringin to prunin by cross-linked naringinase aggregate was investigated. The effects of substrate concentration, pH, temperature, enzyme dosage and the reaction time on the preparation of prunin by cross-linked naringinase aggregates were optimized, and the prunin concentration was took as the optimization index. The orthogonal design was used to optimize the catalytic processes, and the optimum conditions for producing the prunin were as follow: substrate concentration 13.79 mmol/L, pH 8.0, temperature 65 °C, enzyme dosage 18.0 mg/mL, reaction time 12.0 h. Under the above conditions, the production of prunin was about 13.36 mmol/L, and the yield of prunin was 96.87 %. The cross-linked aggregates was stable, it could successively convert for three cycles, and the yield of prunin could reach 91.29 %. Prunin can be effectively separated from the hydrolysis products by using the polyamide resin adsorption and 40% to 60 % isopropanol linear gradient elution .It provided a new approach for preparing the prunin.
MA Huan , CHEN Gang , WANG Tao , LI Qin-geng
2016, 33(3).
Abstract:A synthetic route of water-soluble docetaxel derivative (Ⅰ) was designed. 7, 10-Oxo- dibenzyloxy oxygen acyl-docetaxel (Ⅴ) was obtained through esterification, condensation and selective deprotection of 10-deacetylbaccatin III (Ⅱ) as the starting material. This key intermediate was further reacted with an amino acid, and followed by hydrogenolysis in the presence of palladium on carbon to obtain the target docetaxel derivative (Ⅰ). The structure of product was characterized by means of 1HNMR, 13CNMR and HRMS. The synthetic route was benefited from simple operation, overall yield of 64.1% and purity of over 99% (HPLC).
Tao tingxian , Xu jiabin , chu wei
2016, 33(3).
Abstract:Bi(NO3)3 and Na2MoO4 were used as starting materials, amidoxime fiber as carrier to prepare Bi2MoO6/amidoxime fiber (AOCF) via a facile liquid-phase synthesis approach. The structure and composition of the product were determined by powder X-ray diffraction (XRD), scanning electron microscopy(SEM), and energy dispersive spectrometry(EDS). The results showed that the Bi2MoO6 distributed evenly on the surface of the fiber, and combined with the fiber through coordination bond. The results of photodegrading rhodamine B(Rh B) indicated that Bi2MoO6/AOCF had good photocatalytic activity and the catalytic activity was better in acidic condition. Catalyst also revealed good photocatalytic activity on reactive yellow/methylene blue /methyl orange, and after repeated 5 times for Rh B degradation was still up 91.4%. The photocatalytic reaction accorded with first-order kinetics.
LI Bin , XUE Feng , JU Shen Gui
2016, 33(3).
Abstract:Atipamzole Hydrochloride was synthesized from 2 - (2 - bromine acetyl) - 2 - ethylindanone through three-step reations includingthe imidazole ring formation, carbonyl reduction and hydrochloric acid .The technological conditions of imidazole ring formation were improved, and the effect of reaction temperature on the yield was investigated, Determined the optimum reaction conditions .The yield of the reaction was increased to 72%. In the process of reduction of the carbonyl group, the method of Huang Minglong reduction was used to replace the original palladium carbon reduction method, and the reaction conditions were optimized by orthogonal experiment. The optimum technological conditions were determined
WANG Li , ZHOU HONG WEI , JIANG WEN YUAN , HUANG CHOU , YI YING
2016, 33(3).
Abstract:In order to explore the stabilizing effect of solid particles on the emulsions, nano-silica was synthesized by using L-lysine as the catalyst, and was modified by hexamethyldisilazane in order to obtain hydrophobic performance. Pickering emulsions were prepared by nano-silica acting as stabilizer which was modified by HMDS. The preparation, surface modification of nano-silica and properties of Pickering emulsions were characterized by particle size analyzer, HRTEM, FTIR,TG-DSC, contact angle, optical microscope and electrical conductivity meter respectively. The results showed that the silica spheres with small particle size and uniform morphology were successfully synthesized, and the hydrophobic bond of trimethylsilyl was successfully grafted onto the surface of nano-silica. For Pickering emulsions prepared by different concentration of nano-silica, the stability of emulsions increased gradually with the increase of concentration of nano-silica. Meanwhile, the droplet diameter of emulsions decreased with the increase of concentration of nano-silica. Pickering emulsions prepared by different oil/water ratio, we can conclude the stability of the emulsions increased with the increase of oil phase volume to some extent.
2016, 33(3).
Abstract:Quinoidal π-conjugation usually possess long-wavelength absorption and multistage redox properties which make it as promising organic electronic materials. In addition, incorporating heteroatoms into conjugated skeleton is an intriguing target because the introduction of heteroatoms would induce a variety of intermolecular interactions, such as van der Waals interactions and heteroatom-heteroatom interactions (S • • •S or Se• • • Se interactions), which is essential to achieve highly ordered supramolecular self-assembled structure and eventually excellent device performance. Herein, a facile route has been developed for the preparation of meso-position sulfur embedded quinoidal bisanthene 1. Thione 3 were prepared from corresponding thioxanthen-9-one via reaction with Lawesson’s reagent followed by the Barton-Kellogg reaction with 9-diazothioxanthene derived from corresponding hydrazine to afford the thioepoxides 5. The resulting compound 5 were then treated with copper powder to give the desired olefin precursor 6. Katz-modified Mallory photocyclization was carried out on 6 for the purpose to obtain the target molecule 1. The reaction was conducted by irradiation of the benzene solution of 6 with a 450 W medium-pressure mercury vapor lamp in the presence of I2 and propylene oxide. Unfortunately, only the partially cyclized product 7 were obtained in 77% yield. The reason leading to this result is that there is no more stilbene structure in compound 7. This partially cyclized product 7 showed extended π-conjugation compared with its olefin precursors 6 and exhibited 105 nm and 90 nm red shift of the corresponding absorption maxima and emission maxima. In addition, compound 7 can be oxidized into charged states which are stabilized by the delocalized π-system.
Shan Bin , Tang Bingtao , Liu Yanan , Zhang Shufen
2016, 33(3).
Abstract:The low molecular weight polymer of poly(N-vinylformamide) was synthesized by precipitation polymerization in N,N-dimethyl formamide and ethyl acetate, using azobisisbutyronitrile as the free radical initiator and dodecyl mercaptan as the chain transfer agent. The influences of monomer mass fraction, component solvent ratio, initiator concentration, chain transfer agent concentration, reaction temperature and time on the precipitation polymerization were investigated. In the optimum conditions, the polymer was obtained with 93.1% yield and the number average molecular weight (Mn) of the polymer was 2975.2 with PDI of 2.64 and the polymerization residue could be recycled . Then the polymer was hydrolyzed to poly(N-vinylformamide-co-vinylamine) with different amination degree in the hydrochloric acid solution. The hydrolysis products with the number average molecular weight of 1000~1400 and PDI of 1.34~1.40 were obtained.
2016, 33(3).
Abstract:Chitosan coated humic acid (CTS/HA) microcapsules as a new kind of water retention materials were prepared using chitosan (CTS) as wall materials and humic acid (HA) as the cores. The structure and surface morphology of CTS/HA were characterized and observed by fourier transform infrared Spectrum (FTIR), polarizing microscope (POM) and scanning electron microscope (SEM), respectively. The influences of m(CTS)/m(HA), curing agent content and stirring rate were discussed on the surface morphology of microcapsules, and the water-retention of CTS/HA was also tested. The results showed that CTS/HA displayed good surface morphology microcapsule when the m(CTS)/m(HA) was 1:3, the content of curing agent was 1% of the total mass for CTS/HA and the stirring rate was 500 r/min. In addition, the microcapsule had good water absorption and water retention performance with water absorption rate and water retention rate as high as 248% and 158% in 12 h, respectively.
2016, 33(3).
Abstract:Graphene oxide (GO) was firstly prepared from modified Hummers method, then silanized GO is reduced in situ emulsion using aqueous ammonia to achieve reduced graphene oxide/waterborne polyurethane (KRGO/WPU) nanocomposites.The effect of KRGO content on the fracture morphologies, mechanical performance, thermal stability and water-retardant properties of KRGO/WPU composites was investigated by FT-IR,XRD,TEM, SEM, universal testing machine, TG etc. The results showed that the thermal stability of KRGO/WPU is obviously higher than pure WPU, and the effect of thermal stability decreases with the increase content of KRGO. When the KRGO is up to 1.0wt%, the tensile strength of the composite reached its maxmum 20.2 MPa, 187.1% higher than that of pure WPU.However, the effects were less pronounced at high content (2.0wt%) due to the agglomeration of KRGO particles.In addition, the stability and water-retardant property of KRGO/WPU composites is obviously improved compared with pure WPU.
NI Mao-jun , Bao Wen Ting , Chen Zhu Ping
2016, 33(3).
Abstract:PVA/PVP/ collagen composite hydrogel with high biological activity was prepared by a combination of irradiation crosslinking and freezing/ thawing cycles. The effect of PVP content and collagen on water content, swelling property and mechanical property of the hydrogel were studied. The biocompatibility of PVA/PVP and PVA/PVP/collagen hydrogel was tested by MTT. The results showed that PVA/PVP/collagen hydrogel scaffolds with high swelling property can be obtained by the combination of radiation crosslinking and freezing/ thawing cycles. Collagen was helpful to improve the swelling performance of PVA/PVP hydrogel while the mechanical property was decreased. Biocompatibility study showed that PVA/PVP/collagen hydrogel had better biocompatibility compared with the PVA/PVP hydrogel, and was more conducive to promote cell growth.
WANG Ling , LI Sha , ZHANG Ai-ping
2016, 33(3).
Abstract:TiO2/N-succinyl-chitosan composite was prepared by compositing TiO2 and N-succinyl-chitosan. The composite was characterized by transmission electron microscopy (TEM), fourier infrared spectrum (FTIR), ultraviolet-visible spectra (UV-Vis), X-ray diffraction (XRD), particle size and Zeta potential analysis. The results showed that stable composite was formed by interaction of the surface hydroxyl groups of TiO2 with hydroxyl, amide and carboxyl groups of N-succinyl-chitosan. TiO2 of the composite was anatase. The average particle size of the composite was 50 nm and Zeta potential was 39 mV. Ultraviolet-visible spectra revealed that light response range of the composite was widened to visible region and the light absorption capacity significantly enhanced, but its photocatalytic efficiency was lower than TiO2 under simulated sunlight.
JIANG Yan-wei , LIANG rong , CAO Guang-qun
2016, 33(3).
Abstract:The stable Pickering emulsions were prepared from starch nanocrystals (SNC) combined with cationic quaternized chitosan(QCS). And the properties of aqueous dispersion of QCS/SNC and Pickering emulsions were characterized by Fourier transform infrared spectroscopy( FT-IR), surface/interfical tensiometer, rheometer, optical microscope and fluorescence microscope. The results showed that QCS was absorbed on the surface of SNC through hydrogen-bonding interaction and electrical attraction. The dispersion of emulsifier was improved and the surface tension and interfacial tension of the SNC suspension aqueous decreased by the addition of QCS. With the increasing of the mass fraction of QCS, the droplet size of emulsion increased firstly, but decreased then, eventually increased again. When the mass fraction of QCS was 0.4%, the smallest droplet of emulsions was acquired, and the creaming would be not occurred even after a period of 30d storage at room temperature.
YANG Ming-ming , LIU Wen-lei , ZHANG Yan , CHEN Chun-yan , XIAO Ze-yi
2016, 33(3).
Abstract:Strain Pseudomonas aeruginosa BC1 was cultured in the fermentation coupling with pervaporation (FCP) system and the fed-batch fermentation system separately for production of rhamnolipids and the two fermentation process each lasted for 124h and 107h respectively. In the FCP system, the maximum optical density OD600 of the biomass was 1.06; maximum optical density OD600 of biosurfactant was 0.61; meanwhile, the total rhamnolipids concentration was quantified as 1.3g/L, which was 38% more than that in the fed-batch fermentation system; in the 29th hour of the FCP process, the surface tension of the fermentation supernatant was 22.56mN/m, as a contrast, the surface tension of pure water was 67.52mN/m. Furthermore, the fermentation supernatant showed excellent emulsifying ability to liquid paraffin, motor oil, diesel oil, n-hexane and hexadecane. The permeation vapor was analyzed by gas chromatography mass spectrometry (GC-MS) coupling with solid-phase micro-extraction (SPME) and several volatile organic compounds were detected, including ethanol, pentanol etc. The data indicate that, in contrast to the fed-batch system, the FCP system can increase the cell concentration and the rhamnolipids production through removing growth inhibition of cells from some volatile metabolites produced in the fermentation process.
QU Guang-miao , XUE Chun-long , CHENG Jie-cheng , HAN Ying , LIANG Shuang , DING Wei
2016, 33(3).
Abstract:The aggregation structure of surfactant 2,3-dimethyl-5- (5'-16 alkyl) benzene sulfonate (C16-5OXS) at the oil/water interface was investigated by union atom molecular dynamics simulation. The effect of weak alkaline Na2CO3 on the aggregation behavior of C16-5OXS molecules was also investigated. The results showed that C16-5OXS can form a monolayer at the oil/water interface. With the increase of the concentrations of Na2CO3, the thickness of the interfacial film is decreasing. At low concentrations of Na2CO3, The thickness of the electric double layer of C16-5OXS has little change. But the thickness of the fixed layer sudden drop from 0.106nm to 0.082nm.when the concentrations of Na2CO3 is 1.2 %, at the same time, hydrophilic area decline constantly. C16-5OXS can form a closed packed monolayer at the oil/water interface. The decline of order parameter of hydrophobic chain atoms showed that the conformation of hydrophobic chain will change with the addition of Na2CO3. Research the mechanism of action between Na2CO3 and C16-5OXS at the molecular level.
2016, 33(3):0-0.
Abstract:Abstract: The method of extraction and purification of 3 nonionic surfactants from Camellia Oleifera Abel meal,Sapindus Mukorossi Gaertn and Gleditsia Sinensis Lam were researched respectively,in addition,the influencing factors of their surfactant activity and their complex synergism were evaluated as well .The experimental results show that,after extraction and purification,the surfactant activity of the final extracts were obviously superior to the original natural materials. The influence factors on surfactant activity also showed that their surfactivity were enhanced while in acidic conditions, high temperature and binary mixed systems ,but the effects of salinity and the hardness of water on their surfactivity were not obvious. Results showed that while the extracts were compounded in the proportion which calculated and conclued based on Rosen theory, the ability of m(Sapindus Mukorossi Gaertn extracts):m(Gleditsia Sinensis Lam extracts)=1.58:1.00system (systemIII) to form micelles increaed by 76% than the single component while the ability of m(Camellia Oleifera Abel meal extracts) : m(Gleditsia Sinensis Lam extracts)=1.90:1.00 system (systemII)to reduce the surface tension enhanced by 10.5%,which indicated both of them have synergistic effect .Furthermore,the results of foam property testing indicated that ,compared with the single component,the binary mixed systems showed excellent foam property, especially the m(Sapindus Mukorossi Gaertn extracts):m(Gleditsia Sinensis Lam extracts)=1.58:1.00 system(system III) performed best.
2016, 33(3).
Abstract:Traditional sulfonated melamine resin (SMF) as high-range water-reducer easily causes a big slump loss and high bleeding ratio of concrete, sodium lignosulfonate grafting melamine resin (SLMF) was synthesized with (NH4)2S2O8 as the radical initiator, and the optimal process variables were obtained. Both of the results of IR and the properties of SLMF showed that sodium lignosulfonate was successfully grafted into SMF. SLMF synthesized under the optimal process variables had good properties of dispersion effect and water retention. When the mass ratio of water to cement was 0.29, the fluidity of cement paste with the addition of 0.6% (mass fraction) of SLMF was 253mm. The fluidity loss within 90 min and the water bleeding ratio within 140min decreased to 61.8% and 1.61% from 100% and 4.84%, respectively. The results indicate that SLMF overcomes the shortages of SMF, and hence exhibits potential application in high-range water-reducer.
2016, 33(3).
Abstract:With fumaric acid and ammonium hydroxide as raw materials, synthesis of L-aspartic acid by immobilized cells of aspartase engineering bacteria was carried out. The effect of fumaric acid concentration, pH and reaction temperature was investigated. The optimized preparation conditions were as follows: 300 g/L fumaric acid, 37oC, pH7.5, the yield of L-aspartic acid is 96.7%. The immobilized bacteria could be used continuously for 10 times. The aspartase engineering bacterias were distributed evenly over the carrier by electron microscope.The immobilized cells of aspartase engineering bacterias have good stability.
WANG Meng , YANG Qian-xu , YANG Ying , CHEN Wei , ZHU Bao-kun
2016, 33(3).
Abstract:Based on make flavor/aroma quality of cigarette prominent and highlight product styles, aromatic plants Granules were prepared by low-temperature fluidized bed granulation processing. The optimal operational parameters of spray granulation processing of aromatic plants were obtained based on Box-Benhnken experimental design. The plant granules include 30% chamomile, 5% Rosa rugose, 25% Siraitia grosvenorii, 15% rosemary and 5% Pelargoniums mixed with 20% Radix Ophiopogonis, which was added into cigarette filter to improve the style characteristics of fresh smell, sweet scent and flower fragrance. In conclusion, the addition of aromatic plants granule presented as much more aroma amount,good smoke concentration,improved Sensory quality, and Strengthen the Fen-Sweet flavor style characteristics.