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2015 Volume 32 Issue 4
2015, 32(4): 367-378
doi: 10.11944/j.issn.1000-0518.2015.04.140246
Abstract:
Polymeric nanocarriers with controllable drug realease and stimuli-responsive to targeted biological conditions are an advancing and potential carrier candidate for nanomedicines. Hyperbranched polyglycerols(HPG) spur the interest of the biomaterial community due to their well-defined three-dimensional structures,good solubility,high biocompatiblity and multiple attachment sites for modification. Functionally modified HPG derivatives are able to self-assemble into a variety of drug carriers such as micelles and vesicles. Herein,we present the current progress on functional modified HPG for drug delivery with particular focus on amphiphilic modification, stimuli-responsive functionalization, as well as supra molecular self-assembly.Molecular design strategy for HPG modification with amphiphilic and stimuli responsive functionalization is systematically summarized. Furthermore,the assembly behavior of hyperbranched supra molecular polyglycerol copolymers based on cyclodextrin host-guest interactions is also mentioned.
Polymeric nanocarriers with controllable drug realease and stimuli-responsive to targeted biological conditions are an advancing and potential carrier candidate for nanomedicines. Hyperbranched polyglycerols(HPG) spur the interest of the biomaterial community due to their well-defined three-dimensional structures,good solubility,high biocompatiblity and multiple attachment sites for modification. Functionally modified HPG derivatives are able to self-assemble into a variety of drug carriers such as micelles and vesicles. Herein,we present the current progress on functional modified HPG for drug delivery with particular focus on amphiphilic modification, stimuli-responsive functionalization, as well as supra molecular self-assembly.Molecular design strategy for HPG modification with amphiphilic and stimuli responsive functionalization is systematically summarized. Furthermore,the assembly behavior of hyperbranched supra molecular polyglycerol copolymers based on cyclodextrin host-guest interactions is also mentioned.
2015, 32(4): 379-385
doi: 10.11944/j.issn.1000-0518.2015.04.140253
Abstract:
Several basic physical properties of poly(arylene ether ketone) s containing N-alkylcarbazole(PPCz E,PPCz B and PPCz H) were studied in comparison with the corresponding analog,commercialized phenolphthalein poly(ether ketone)(PEK-C). Strong UV absorption and blue light emission ability are exhibited by these polymers due to the introduction of carbazole structure. The water contact angle of polymers(87°~103°) is greater than that of PEK-C(76°),because of the hydrophobic nature of alkyl groups. While at the same time,these polymers have higher water uptake capabilities than PEK-C which is probably due to their larger chain distance. In addition,these polymers exhibit good dimensional stability(linear thermal expansion coefficient 6.4×10-5℃-1) and electrical insulating(volume resistivity 10sup>16Ω·cm) property. Young's modulus,tensile strength and elongation at break of these polymers are in the range of 1.9~2.0 GPa,72.5~75.0 MP and 6.5%~7.2%,respectively. Dynamic mechanical analysis shows that PPCz E remains good tensile property at the temperature up to 225℃.
Several basic physical properties of poly(arylene ether ketone) s containing N-alkylcarbazole(PPCz E,PPCz B and PPCz H) were studied in comparison with the corresponding analog,commercialized phenolphthalein poly(ether ketone)(PEK-C). Strong UV absorption and blue light emission ability are exhibited by these polymers due to the introduction of carbazole structure. The water contact angle of polymers(87°~103°) is greater than that of PEK-C(76°),because of the hydrophobic nature of alkyl groups. While at the same time,these polymers have higher water uptake capabilities than PEK-C which is probably due to their larger chain distance. In addition,these polymers exhibit good dimensional stability(linear thermal expansion coefficient 6.4×10-5℃-1) and electrical insulating(volume resistivity 10sup>16Ω·cm) property. Young's modulus,tensile strength and elongation at break of these polymers are in the range of 1.9~2.0 GPa,72.5~75.0 MP and 6.5%~7.2%,respectively. Dynamic mechanical analysis shows that PPCz E remains good tensile property at the temperature up to 225℃.
2015, 32(4): 386-391
doi: 10.11944/j.issn.1000-0518.2015.04.140270
Abstract:
The composite polyampholyte hydrogels(CAH) were prepared by inserting core-shell microgel particles into a bulk polyampholyte matrix. CAH gels with uniform and tight network structure have excellent mechanical performance due to the entanglement between microgels and network chains,and exhibit an antipolyelectrolyte effect and pH-sensitivity. And ionic strength drastically affects their swelling behaviors.Meanwhile,CAH gels show rapid shrinking rate and transmittance switch in response to the temperature change as a result of the incorporation of microgel particles.
The composite polyampholyte hydrogels(CAH) were prepared by inserting core-shell microgel particles into a bulk polyampholyte matrix. CAH gels with uniform and tight network structure have excellent mechanical performance due to the entanglement between microgels and network chains,and exhibit an antipolyelectrolyte effect and pH-sensitivity. And ionic strength drastically affects their swelling behaviors.Meanwhile,CAH gels show rapid shrinking rate and transmittance switch in response to the temperature change as a result of the incorporation of microgel particles.
2015, 32(4): 392-398
doi: 10.11944/j.issn.1000-0518.2015.04.140286
Abstract:
With raw materials of benzoyl chloride and p-bromophenol, mono-Schiff base, 2-[(2-aminophenylimino) phenylmethyl]-4-bromophenol,is obtained through multi-step reactions of esterification,Fries rearrangement and condensation. The mono-Schiff base reacts with aldehydes and ketones to give five asymmetric di-Schiff bases and two symmetric di-Schiff bases. These Schiff bases,particularly those containing sulfur atom in the molecule,show good antibacterial activities with a minimum inhibitory concentration of 1×10-4g/L.
With raw materials of benzoyl chloride and p-bromophenol, mono-Schiff base, 2-[(2-aminophenylimino) phenylmethyl]-4-bromophenol,is obtained through multi-step reactions of esterification,Fries rearrangement and condensation. The mono-Schiff base reacts with aldehydes and ketones to give five asymmetric di-Schiff bases and two symmetric di-Schiff bases. These Schiff bases,particularly those containing sulfur atom in the molecule,show good antibacterial activities with a minimum inhibitory concentration of 1×10-4g/L.
2015, 32(4): 399-404
doi: 10.11944/j.issn.1000-0518.2015.04.140359
Abstract:
Seven novel 1,2,4-triazole derivatives containing thioether and thiazole were designed and synthesized from ethyl 4,4,4-trifluoro-3-oxobutanoate, sulfonyl chloride, hydrazine hydrate, phenyl isothiocyanate,aryl iodides,chloroacetic acid as starting materials via substitution,hydrazinolysis,cyclization and Ullmann coupling. The structures of these compounds were characterized with13C NMR,1H NMR,19F NMR and MS. Bactericidal activity test shows that Rhizoctoniasolani can be inhibited by compounds 6b,6d,and 6g at a concentration of 100 mg/L with inhibition rates of 91%,92% and 93%,respectively.
Seven novel 1,2,4-triazole derivatives containing thioether and thiazole were designed and synthesized from ethyl 4,4,4-trifluoro-3-oxobutanoate, sulfonyl chloride, hydrazine hydrate, phenyl isothiocyanate,aryl iodides,chloroacetic acid as starting materials via substitution,hydrazinolysis,cyclization and Ullmann coupling. The structures of these compounds were characterized with13C NMR,1H NMR,19F NMR and MS. Bactericidal activity test shows that Rhizoctoniasolani can be inhibited by compounds 6b,6d,and 6g at a concentration of 100 mg/L with inhibition rates of 91%,92% and 93%,respectively.
2015, 32(4): 405-411
doi: 10.11944/j.issn.1000-0518.2015.04.140251
Abstract:
Using acetone and 2-hydroxybenzaldehyde as starting materials,nine novel curcumin derivatives containing 1,2,4-triazole and amide units were synthesized. The structures were confirmed by 1H NMR,19F NMR,IR and elemental analysis. The preliminary result of bioassay by airbrush spraying shows that some of the compounds obtianed exhibit weak to moderate insecticidal activity.
Using acetone and 2-hydroxybenzaldehyde as starting materials,nine novel curcumin derivatives containing 1,2,4-triazole and amide units were synthesized. The structures were confirmed by 1H NMR,19F NMR,IR and elemental analysis. The preliminary result of bioassay by airbrush spraying shows that some of the compounds obtianed exhibit weak to moderate insecticidal activity.
2015, 32(4): 412-415
doi: 10.11944/j.issn.1000-0518.2015.04.140294
Abstract:
4-Hydroxyl-2-(methylsulfanyl)-pyrimidine-5-carboxylic acid ethyl ester was synthesized from S-methylisothiourea hemisulfate salt and diethyl ethoxymethylenemalonate in ethanol. The feed ratio,reaction temperature,reaction time and other factors were optimized to improve the yield. The 81.1% yield of white solid product is obtained when the sodium hydroxide solution is dropwisely added into the reaction mixture in a molar ration of n(C2H6N2S·1/2H2SO4):n(C10H16O5):n(NaOH)=1.2:1:1.8 under stirring at room temperature for 6 h then with acid treatment. Its structure was characterized by melting point,1H NMR,ESIMS and FT-IR.
4-Hydroxyl-2-(methylsulfanyl)-pyrimidine-5-carboxylic acid ethyl ester was synthesized from S-methylisothiourea hemisulfate salt and diethyl ethoxymethylenemalonate in ethanol. The feed ratio,reaction temperature,reaction time and other factors were optimized to improve the yield. The 81.1% yield of white solid product is obtained when the sodium hydroxide solution is dropwisely added into the reaction mixture in a molar ration of n(C2H6N2S·1/2H2SO4):n(C10H16O5):n(NaOH)=1.2:1:1.8 under stirring at room temperature for 6 h then with acid treatment. Its structure was characterized by melting point,1H NMR,ESIMS and FT-IR.
2015, 32(4): 416-421
doi: 10.11944/j.issn.1000-0518.2015.04.150040
Abstract:
In order to increase the yield and optimize the process of preparation for cloquintocet-mexyl in industrial,the synthesis of cloquintocet-mexyl in this paper was investigated using 5-chloro-8-hydroxyquinoline and methylhexyl chloroacetate as raw materials. The alkali used in the reaction,reaction time,the molar ratio of 5-chloro-8-hydroxyquinoline to methylhexyl chloroacetate and the molar ratio of potassium carbonate to methylhexyl chloroacetate were determinated. The kinetic equation for this reaction was established. The result shows that the synthesis of cloquintocet-mexyl is a second-order reaction. The kinetics experiments were carried out at 323 K,328 K,333 K,339 K,respectively. The frequency factor is 49.82 kJ/mol and the activation energy is 49.82 kJ/mol which are obtained from the reaction rate constants at different temperatures by using the Arrhenius equation. The reaction kinetic equation is -r2=-(dc2)/(dt)=1.46×108e(-49.82×103/RT)c1c2.It provides the basic data for the industrial development of cloquintocet-mexyl.
In order to increase the yield and optimize the process of preparation for cloquintocet-mexyl in industrial,the synthesis of cloquintocet-mexyl in this paper was investigated using 5-chloro-8-hydroxyquinoline and methylhexyl chloroacetate as raw materials. The alkali used in the reaction,reaction time,the molar ratio of 5-chloro-8-hydroxyquinoline to methylhexyl chloroacetate and the molar ratio of potassium carbonate to methylhexyl chloroacetate were determinated. The kinetic equation for this reaction was established. The result shows that the synthesis of cloquintocet-mexyl is a second-order reaction. The kinetics experiments were carried out at 323 K,328 K,333 K,339 K,respectively. The frequency factor is 49.82 kJ/mol and the activation energy is 49.82 kJ/mol which are obtained from the reaction rate constants at different temperatures by using the Arrhenius equation. The reaction kinetic equation is -r2=-(dc2)/(dt)=1.46×108e(-49.82×103/RT)c1c2.It provides the basic data for the industrial development of cloquintocet-mexyl.
2015, 32(4): 422-427
doi: 10.11944/j.issn.1000-0518.2015.04.140313
Abstract:
Cinchona alkaloid derivatives as organocatalysts were applied in asymmetric Michael addition reaction of anthrone with various trans-β-nitroolefins. Solvent,temperature and catalyst loading were screened.The optimized conditions are using toluene as the solvent with a 5%( molar fraction) loading of catalyst 1b at room temperature. The products are obtained in 91%~99% yield with up to 95% ee.
Cinchona alkaloid derivatives as organocatalysts were applied in asymmetric Michael addition reaction of anthrone with various trans-β-nitroolefins. Solvent,temperature and catalyst loading were screened.The optimized conditions are using toluene as the solvent with a 5%( molar fraction) loading of catalyst 1b at room temperature. The products are obtained in 91%~99% yield with up to 95% ee.
2015, 32(4): 428-432
doi: 10.11944/j.issn.1000-0518.2015.04.140298
Abstract:
Carbon supported Pd/Ce bimetallic catalyst was prepared readily for Heck reaction. The effect of reaction conditions on the catalytic properties of carbon supported Pd/Ce bimetallic catalyst was studied in details with the model Heck reaction of iodobenzene and acrylic acid. The results show that carbon supported Pd/Ce bimetallic catalyst can effectively catalyze the Heck reactions under the conditions of 130℃,5 h,DMF as the solvent,and Bu3 N as the base to afford the product with a yield of over 70%. Additionally,the heterogeneous carbon supported Pd/Ce bimetallic catalyst can be easily separated from the reaction solution.Furthermore,the catalyst can be reused for 3 times with a yield of 69% and without the significant loss of catalytic efficiency.
Carbon supported Pd/Ce bimetallic catalyst was prepared readily for Heck reaction. The effect of reaction conditions on the catalytic properties of carbon supported Pd/Ce bimetallic catalyst was studied in details with the model Heck reaction of iodobenzene and acrylic acid. The results show that carbon supported Pd/Ce bimetallic catalyst can effectively catalyze the Heck reactions under the conditions of 130℃,5 h,DMF as the solvent,and Bu3 N as the base to afford the product with a yield of over 70%. Additionally,the heterogeneous carbon supported Pd/Ce bimetallic catalyst can be easily separated from the reaction solution.Furthermore,the catalyst can be reused for 3 times with a yield of 69% and without the significant loss of catalytic efficiency.
2015, 32(4): 433-441
doi: 10.11944/j.issn.1000-0518.2015.04.140277
Abstract:
An inorganic-organic hybrid compound[Cu(H2biim)2(H2O)] [{ Cu(H2biim)2}2(P2W18O62)]·11H2O(H2biim=2,2'-biimidazole)(1) has been hydrothermally constructed by the reaction of Cu(Ⅱ)-H2 biim complexes and Dawson-type tungstophosphate,and characterized by single-crystal X-ray diffraction,infrared spectroscopy(IR),X-ray powder diffraction(XRD),elemental analysis and electrochemical analysis.Structural analysis shows that the polyanion[P2W18O62]6-,as a bidentate ligand,coordinates with two Cu2+ ions to form a bi-Cu(Ⅱ)-supporting heteropolyanion[{ Cu(H2biim)2}2(P2W18O62)]2-,which is surrounded by an isolated[Cu(H2biim)2(H2O)]2+ and eleven H2O molecules. The presence of N-H…O/OW hydrogen bonds between H2biimmolecules and polyoxoanion or water molecules,in company with the synergistic effect of electrostatic interactions and π-π stack,leads to the formation of a crystal material with 3D framework further. Compound 1 displays good electrocatalytic activity toward the reduction of H2O2 and Na2NO2.Meanwhile it is also a good acid-catalyst for the synthesis of cyclohexanone ethylene ketal and can be recycled.
An inorganic-organic hybrid compound[Cu(H2biim)2(H2O)] [{ Cu(H2biim)2}2(P2W18O62)]·11H2O(H2biim=2,2'-biimidazole)(1) has been hydrothermally constructed by the reaction of Cu(Ⅱ)-H2 biim complexes and Dawson-type tungstophosphate,and characterized by single-crystal X-ray diffraction,infrared spectroscopy(IR),X-ray powder diffraction(XRD),elemental analysis and electrochemical analysis.Structural analysis shows that the polyanion[P2W18O62]6-,as a bidentate ligand,coordinates with two Cu2+ ions to form a bi-Cu(Ⅱ)-supporting heteropolyanion[{ Cu(H2biim)2}2(P2W18O62)]2-,which is surrounded by an isolated[Cu(H2biim)2(H2O)]2+ and eleven H2O molecules. The presence of N-H…O/OW hydrogen bonds between H2biimmolecules and polyoxoanion or water molecules,in company with the synergistic effect of electrostatic interactions and π-π stack,leads to the formation of a crystal material with 3D framework further. Compound 1 displays good electrocatalytic activity toward the reduction of H2O2 and Na2NO2.Meanwhile it is also a good acid-catalyst for the synthesis of cyclohexanone ethylene ketal and can be recycled.
2015, 32(4): 442-446
doi: 10.11944/j.issn.1000-0518.2015.04.140235
Abstract:
By partially substituting of CaO with CaF2,in CaO-P2O5-SiO2-Na2O-B2O3glass-ceramic system a new precursor powder was prepared by the sol-gel method. Its crystallization temperature was determined by TG-DSC at 865℃. The main crystal phase of the glass-ceramics is Na6Ca3Si6O18. The microstructures and properties of this glass-ceramics were characterized by X-ray diffractometry(XRD),Fourier transform infrared spectroscopy(FTIR),scanning electron microscopy(SEM) and in vitro assays. By addition of CaF2,the volume density,bending strength and microhardness of the glass-ceramics are significantly improved,but the bioiogical activity of the glass-ceramics is maintained.
By partially substituting of CaO with CaF2,in CaO-P2O5-SiO2-Na2O-B2O3glass-ceramic system a new precursor powder was prepared by the sol-gel method. Its crystallization temperature was determined by TG-DSC at 865℃. The main crystal phase of the glass-ceramics is Na6Ca3Si6O18. The microstructures and properties of this glass-ceramics were characterized by X-ray diffractometry(XRD),Fourier transform infrared spectroscopy(FTIR),scanning electron microscopy(SEM) and in vitro assays. By addition of CaF2,the volume density,bending strength and microhardness of the glass-ceramics are significantly improved,but the bioiogical activity of the glass-ceramics is maintained.
2015, 32(4): 447-452
doi: 10.11944/j.issn.1000-0518.2015.04.140242
Abstract:
A series of Li+ and Eu3+ co-doped red phosphors La1.9-xMoO6:0.10Eu3+,xLi+(x=0,0.10,0.20,0.25) has been successfully synthesized via Pechiini method. And the samples were investigated by the X-ray diffraction(XRD),scanning electron microscope(SEM),energy dispersive spectrometer(EDS) and photoluminescence(PL) measurements. The PL results reveal that the samples can be excited efficiently by near-ultraviolet(near-UV)(395 nm) and blue light(466 nm),and exhibit strong red emission peaks at 616 nm and 623 nm,due to the5D0→7F2 electric dipole transition of Eu3+. These phosphors exhibit potential commercial value since they match well with white light emitting diode(W-LED) near-UV chip(370~410 nm) and blue light chip(450~470 nm). Addition of Li+ acting as a sensitizer strongly enhances the emission intensity of the phosphors,and the optimum concentration is x=0.20.
A series of Li+ and Eu3+ co-doped red phosphors La1.9-xMoO6:0.10Eu3+,xLi+(x=0,0.10,0.20,0.25) has been successfully synthesized via Pechiini method. And the samples were investigated by the X-ray diffraction(XRD),scanning electron microscope(SEM),energy dispersive spectrometer(EDS) and photoluminescence(PL) measurements. The PL results reveal that the samples can be excited efficiently by near-ultraviolet(near-UV)(395 nm) and blue light(466 nm),and exhibit strong red emission peaks at 616 nm and 623 nm,due to the5D0→7F2 electric dipole transition of Eu3+. These phosphors exhibit potential commercial value since they match well with white light emitting diode(W-LED) near-UV chip(370~410 nm) and blue light chip(450~470 nm). Addition of Li+ acting as a sensitizer strongly enhances the emission intensity of the phosphors,and the optimum concentration is x=0.20.
2015, 32(4): 453-457
doi: 10.11944/j.issn.1000-0518.2015.04.140260
Abstract:
Silver loaded montmorillonite(Ag-MMT) was prepared by ion-exchange and triethanolamine reduction two-step approach using[Ag(NH3)2OH] as the precursor for silver oxide and ammonia. The silver content in Ag-MMT was determined by the Volhard method. The effects of reaction temperature on silver loading,its release properties,and the structures of Na-MMT and Ag-MMT were characterized by FI-IR and XRD,respectively. The results show that the amount of silver loaded on the montmorillonite is maximum,the utilization rate of silver reaches up to 86.9% and the layered structure of MMT is remained under the optimized conditions:the mass ratio of montmorillonite to Ag+ is 20:1,the ion exchange time is 1 h,and the reaction temperature is 50℃,then triethanolamine and polyvinylpyrrolidone are added and react for 2 h at temperature of 50℃.
Silver loaded montmorillonite(Ag-MMT) was prepared by ion-exchange and triethanolamine reduction two-step approach using[Ag(NH3)2OH] as the precursor for silver oxide and ammonia. The silver content in Ag-MMT was determined by the Volhard method. The effects of reaction temperature on silver loading,its release properties,and the structures of Na-MMT and Ag-MMT were characterized by FI-IR and XRD,respectively. The results show that the amount of silver loaded on the montmorillonite is maximum,the utilization rate of silver reaches up to 86.9% and the layered structure of MMT is remained under the optimized conditions:the mass ratio of montmorillonite to Ag+ is 20:1,the ion exchange time is 1 h,and the reaction temperature is 50℃,then triethanolamine and polyvinylpyrrolidone are added and react for 2 h at temperature of 50℃.
2015, 32(4): 458-463
doi: 10.11944/j.issn.1000-0518.2015.04.140266
Abstract:
In order to alleviate the situation of the country' s reliance on importing high-performance copper foil,the experiment was carried out by introducing metalloid(P) and rare earth(La) in the Zn-Ni alloy coating to obtain high corrosion resistance for the copper foil. The quality of the copper foil coating was characterized by the X-ray photoelectron spectrscopy(XPS),powder X-ray diffraction(XRD) and scanning electron microscope(SEM). Zn-Ni-P-La amorphous alloy coating with well-distributed and dense crystallization was achieved by optimizing the experimental process parameters. The unpassivated copper foil can keep color for one hour in a 180 degree oven and exhibits good antioxidation and anticorrosion abilities. It indicates that a proper amount of P and La in the coating plays an important role in improving the quality of the copper foil coating,which has a good industrial application prospect.
In order to alleviate the situation of the country' s reliance on importing high-performance copper foil,the experiment was carried out by introducing metalloid(P) and rare earth(La) in the Zn-Ni alloy coating to obtain high corrosion resistance for the copper foil. The quality of the copper foil coating was characterized by the X-ray photoelectron spectrscopy(XPS),powder X-ray diffraction(XRD) and scanning electron microscope(SEM). Zn-Ni-P-La amorphous alloy coating with well-distributed and dense crystallization was achieved by optimizing the experimental process parameters. The unpassivated copper foil can keep color for one hour in a 180 degree oven and exhibits good antioxidation and anticorrosion abilities. It indicates that a proper amount of P and La in the coating plays an important role in improving the quality of the copper foil coating,which has a good industrial application prospect.
2015, 32(4): 464-471
doi: 10.11944/j.issn.1000-0518.2015.04.140292
Abstract:
The inhibition effect and adsorption behavior of 1-phenylaminomethylbenzimidazole(PAB) for N80 steel in HCl solution were investigated by mass-loss test,potentiodynamic polarization and electrochemical impedance spectroscopy(EIS). The inhibition efficiency increased with higher concentration of PAB and decreased with elevated temperature. Polarization curve reveals that PAB is a mix-type inhibitor. The adsorption between PAB and N80 steel surface is a spontaneous,exothermic and entropy increasing process fitting Langmuir isotherm. The relationship between the molecular structure of PAB and the inhibition efficiency was investigated using quantum chemical calculations.
The inhibition effect and adsorption behavior of 1-phenylaminomethylbenzimidazole(PAB) for N80 steel in HCl solution were investigated by mass-loss test,potentiodynamic polarization and electrochemical impedance spectroscopy(EIS). The inhibition efficiency increased with higher concentration of PAB and decreased with elevated temperature. Polarization curve reveals that PAB is a mix-type inhibitor. The adsorption between PAB and N80 steel surface is a spontaneous,exothermic and entropy increasing process fitting Langmuir isotherm. The relationship between the molecular structure of PAB and the inhibition efficiency was investigated using quantum chemical calculations.
2015, 32(4): 472-480
doi: 10.11944/j.issn.1000-0518.2015.04.140254
Abstract:
A novel magnetic nonylphenol molecularly imprinted composite extraction materials(MWNTs@Fe3O4-MIPs) was prepared based on multiwalled carbon nanotubes(MWNTs) using nonylphenol(NP) as the template,methacrylic acid(MAA) as the functional monomer and ethylene glycol dimethacrylate(EGDMA) as the cross-linker. The MWNTs@Fe3O4-MIPs were characterized by scanning electron microscopy(SEM),Fourier-transform infrared(FT-IR) analysis and vibrating sample magnetometer(VSM).The results show that a thermally stable magnetic imprinted layer with the thickness of 60~70 nm was coated steadily on the MWNTs surface. Adsorption performance of the MWNTs@Fe3O4-MIPs was investigated by magnetic solid phase extraction(M-SPE) and high-performance liquid chromatography(HPLC) technology.The results indicate that the MWNTs@Fe3O4-MIPs possessed higher selectivity towards nonylphenol(NP) with the maximum adsorption capacity of 38.46 mg/g. This magnetic molecularly imprinted composite material combining with HPLC technology is successfully applied to the separation and the enrichment of nonylphenol(NP) in environmental water samples.
A novel magnetic nonylphenol molecularly imprinted composite extraction materials(MWNTs@Fe3O4-MIPs) was prepared based on multiwalled carbon nanotubes(MWNTs) using nonylphenol(NP) as the template,methacrylic acid(MAA) as the functional monomer and ethylene glycol dimethacrylate(EGDMA) as the cross-linker. The MWNTs@Fe3O4-MIPs were characterized by scanning electron microscopy(SEM),Fourier-transform infrared(FT-IR) analysis and vibrating sample magnetometer(VSM).The results show that a thermally stable magnetic imprinted layer with the thickness of 60~70 nm was coated steadily on the MWNTs surface. Adsorption performance of the MWNTs@Fe3O4-MIPs was investigated by magnetic solid phase extraction(M-SPE) and high-performance liquid chromatography(HPLC) technology.The results indicate that the MWNTs@Fe3O4-MIPs possessed higher selectivity towards nonylphenol(NP) with the maximum adsorption capacity of 38.46 mg/g. This magnetic molecularly imprinted composite material combining with HPLC technology is successfully applied to the separation and the enrichment of nonylphenol(NP) in environmental water samples.
2015, 32(4): 481-488
doi: 10.11944/j.issn.1000-0518.2015.04.140281
Abstract:
In pH 3.4~3.9 Britton-Robinson(BR) buffer solution,mebendazole(MBZ) reacts with eosin Y(EY) to form a 1:1 ion-association complex,which not only results in the quenching of fluorescence,but also results in the great enhancement of resonance Rayleigh scattering(RRS) and frequency doubling scattering(FDS). Furthermore,a new RRS spectrum appears,and the maximum RRS wavelength is located at 326 nm.The detection limit for MBZ is 32.31 μg/L using the fluorophotometry,7.24 μg/L by the RRS method and11.65 μg/L by the FDS method. Among them,the RRS method has the highest sensitivity. The experimental conditions were optimized and effects of coexisting substances were evaluated. These methods have been applied to the determination of MBZ in tablets and human urine samples. The composition and structure of the ion-association complex and the reaction mechanism are discussed.
In pH 3.4~3.9 Britton-Robinson(BR) buffer solution,mebendazole(MBZ) reacts with eosin Y(EY) to form a 1:1 ion-association complex,which not only results in the quenching of fluorescence,but also results in the great enhancement of resonance Rayleigh scattering(RRS) and frequency doubling scattering(FDS). Furthermore,a new RRS spectrum appears,and the maximum RRS wavelength is located at 326 nm.The detection limit for MBZ is 32.31 μg/L using the fluorophotometry,7.24 μg/L by the RRS method and11.65 μg/L by the FDS method. Among them,the RRS method has the highest sensitivity. The experimental conditions were optimized and effects of coexisting substances were evaluated. These methods have been applied to the determination of MBZ in tablets and human urine samples. The composition and structure of the ion-association complex and the reaction mechanism are discussed.
