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2010 Volume 27 Issue 12
2010, 27(12): 1365-1371
doi: 10.3724/SP.J.1095.2010.00171
Abstract:
Single-molecule magnets(SMMs) continue to be an attractive research field because of their potential applications in quantum information storage and quantum computing. Lanthanide-based polynuclear system is an important avenue to explore in pursuit of SMMs with higher anisotropic barriers. The progress and prospect on pure 4f SMMs are briefly reviewed with an emphasis on the magnetic properties of the mono-,tri-and tetra-nuclear dysprosium SMMs.
Single-molecule magnets(SMMs) continue to be an attractive research field because of their potential applications in quantum information storage and quantum computing. Lanthanide-based polynuclear system is an important avenue to explore in pursuit of SMMs with higher anisotropic barriers. The progress and prospect on pure 4f SMMs are briefly reviewed with an emphasis on the magnetic properties of the mono-,tri-and tetra-nuclear dysprosium SMMs.
2010, 27(12): 1372-1375
doi: 10.3724/SP.J.1095.2010.00073
Abstract:
The copolymerization of propylene oxide(PO) with CO2 and homopolymerization of PO catalyzed by double metal cyanide(DMC) catalyst were investigated with focus on the reaction induced period.The results showed that the copolymerization initiated by DMC catalysts has shorter induced period than that of PO homopolymerization.At low pressure(1.0 MPa) of CO2,the induction period of homopolymerization was shorten from 45 min to 15 min.The initiation time prolongs with the increase of,the induction period,and increases from 15 min for copolymerization to 40 min for homopolymerization with enhancing the CO2 pressure from 1.0 to 7.0 MPa,respectively.The induction phenomenon of copolymerization differs dramatically from that of homopolymerization.For the former case,the pressure and temperature experience a sudden abnormal increase and then rapidly return to the state before induction.While in homopolymerization process,the temperature will slowly dropped after a sudden increase occurred in the induction period.Those observations suggest that CO2 can promote the activation of the DMC catalysts.
The copolymerization of propylene oxide(PO) with CO2 and homopolymerization of PO catalyzed by double metal cyanide(DMC) catalyst were investigated with focus on the reaction induced period.The results showed that the copolymerization initiated by DMC catalysts has shorter induced period than that of PO homopolymerization.At low pressure(1.0 MPa) of CO2,the induction period of homopolymerization was shorten from 45 min to 15 min.The initiation time prolongs with the increase of,the induction period,and increases from 15 min for copolymerization to 40 min for homopolymerization with enhancing the CO2 pressure from 1.0 to 7.0 MPa,respectively.The induction phenomenon of copolymerization differs dramatically from that of homopolymerization.For the former case,the pressure and temperature experience a sudden abnormal increase and then rapidly return to the state before induction.While in homopolymerization process,the temperature will slowly dropped after a sudden increase occurred in the induction period.Those observations suggest that CO2 can promote the activation of the DMC catalysts.
2010, 27(12): 1376-1380
doi: 10.3724/SP.J.1095.2010.00147
Abstract:
Crosslinked polystyrene microspheres(CPS) were first chloromethylated with non-carcinogenic 1,4-bis(chloromethoxy) butane(BCMB) to form chloromethylated microspheres(CMCPS).Then quaternization reaction between CMCPS microspheres and 4-pyridylaldehyde was carried out to modify the CPS microspheres with 4-pyridylaldehyde(PyAL-CPS).The effects of main factors on the quaternization reaction were examined,and the synthetic conditions were optimized. The suitable temperature and appropriate solvent are 60℃ and CCl4,respectively. Finally,Alder reaction at the interface of solid/solution between 4-pyridylaldehyde on the surface of modified microspheres and pyrrole was performed to form the functional microspheres(PyP-CPS),on which the formation of pyridyl porphyrin(PyP) could be achieved. The PyP-CPS formation were characterized by using IR and UV-Vis while and the loading of PyP was demonstrated by forming Zn-PyP complex.
Crosslinked polystyrene microspheres(CPS) were first chloromethylated with non-carcinogenic 1,4-bis(chloromethoxy) butane(BCMB) to form chloromethylated microspheres(CMCPS).Then quaternization reaction between CMCPS microspheres and 4-pyridylaldehyde was carried out to modify the CPS microspheres with 4-pyridylaldehyde(PyAL-CPS).The effects of main factors on the quaternization reaction were examined,and the synthetic conditions were optimized. The suitable temperature and appropriate solvent are 60℃ and CCl4,respectively. Finally,Alder reaction at the interface of solid/solution between 4-pyridylaldehyde on the surface of modified microspheres and pyrrole was performed to form the functional microspheres(PyP-CPS),on which the formation of pyridyl porphyrin(PyP) could be achieved. The PyP-CPS formation were characterized by using IR and UV-Vis while and the loading of PyP was demonstrated by forming Zn-PyP complex.
2010, 27(12): 1381-1385
doi: 10.3724/SP.J.1095.2010.00160
Abstract:
Using formaldehyde and melamine as wall materials,encapsulated emamectin benzoate-toluene microcapsules were prepared via an in-situ polymerization process.The experimental results show that well defined microcapsules with uniform particle size around 4.4 μm could be formed when the mass ratio of melamine to formaldehyde is 1:2,core to wall is 3 to 2,using 1% mass fraction of HEC as emulsifying agent,the stirring ratio is 1000 r/min,pH value is 5.0,the temperature and heating time are 50℃ and 2 h,respectively.An improved photodegradation of emamectin benzoate microcapsules toward UV light could be achieved.Fourier-transform infrared spectroscopy(FT-IR) results also demonstrate the successful encapsulation of emamectin benzoate within the wall material.
Using formaldehyde and melamine as wall materials,encapsulated emamectin benzoate-toluene microcapsules were prepared via an in-situ polymerization process.The experimental results show that well defined microcapsules with uniform particle size around 4.4 μm could be formed when the mass ratio of melamine to formaldehyde is 1:2,core to wall is 3 to 2,using 1% mass fraction of HEC as emulsifying agent,the stirring ratio is 1000 r/min,pH value is 5.0,the temperature and heating time are 50℃ and 2 h,respectively.An improved photodegradation of emamectin benzoate microcapsules toward UV light could be achieved.Fourier-transform infrared spectroscopy(FT-IR) results also demonstrate the successful encapsulation of emamectin benzoate within the wall material.
2010, 27(12): 1386-1391
doi: 10.3724/SP.J.1095.2010.00080
Abstract:
An enzymatic synthesis and chemical polymerization strategy has been used to prepare ketoprofen polymeric prodrug with glucose pendant. Polymerizable ketoprofen vinyl ester(KVE) and glucose derivative(6-O-vinylsuccinoyl-D-glucose)(VSUG) were obtained. Then,polymeric prodrugs of ketoprofen were synthesized by the two kinds of monomers with different molar ratios(n(KVE):n (VSUG):1:1,1:2,2:1,4:1) through free radical reaction using AIBN as the initiator. The structures of products were confirmed by IR,NMR,and GPC. The results suggested that the molecular weight decreased and drug loading capacity increased as the ratio of KVE in the feed raised. In vitro release behavior of these copolymers was investigated in PBS(pH=7.4) at 37℃. Contrast to the parent drug,the outcome demonstrated that the polymeric prodrug could effectively prolong the drug release rate. And the release rate of ketoprofen from polymeric prodrugs increased with the raising of glucose in the polymeric prodrug. Furthermore,investigations of the drug release profiles and kinetics suggested that the drug release gave a good fit to first-order kinetic model.
An enzymatic synthesis and chemical polymerization strategy has been used to prepare ketoprofen polymeric prodrug with glucose pendant. Polymerizable ketoprofen vinyl ester(KVE) and glucose derivative(6-O-vinylsuccinoyl-D-glucose)(VSUG) were obtained. Then,polymeric prodrugs of ketoprofen were synthesized by the two kinds of monomers with different molar ratios(n(KVE):n (VSUG):1:1,1:2,2:1,4:1) through free radical reaction using AIBN as the initiator. The structures of products were confirmed by IR,NMR,and GPC. The results suggested that the molecular weight decreased and drug loading capacity increased as the ratio of KVE in the feed raised. In vitro release behavior of these copolymers was investigated in PBS(pH=7.4) at 37℃. Contrast to the parent drug,the outcome demonstrated that the polymeric prodrug could effectively prolong the drug release rate. And the release rate of ketoprofen from polymeric prodrugs increased with the raising of glucose in the polymeric prodrug. Furthermore,investigations of the drug release profiles and kinetics suggested that the drug release gave a good fit to first-order kinetic model.
2010, 27(12): 1392-1395
doi: 10.3724/SP.J.1095.2010.00122
Abstract:
A solvent-free process was developed to synthesize 1,2-epoxycyclopentane(CPEO) from cyclopentene(CPE) using hydrogen peroxide as green oxidant,KCl as cocatalyst and polystyrene-divinylbenzene(PS-DVB) grafted quaternary ammonium phosphor tungsten heterpoly acid salts as tri-phase phase transfer catalysts.Effects of the amount of catalyst and cocatalyst,reaction temperature,reaction time and the molar ratio of CPE to hydrogen peroxide on the product yield were investigated. The suitable reaction conditions with solvent-free were obtained as follows(based on 0.056 mol H2O2):catalyst 1.0 g,cocatalyst 0.025 g,reaction temperature 40℃,reaction time 5h,n(CPE):n(H2O2)=2.1:1.0. Under these conditions,the average yield of CPEO was about 96%. The catalysts can be recovered and even reused for six times without significant decrease of catalytic activity.
A solvent-free process was developed to synthesize 1,2-epoxycyclopentane(CPEO) from cyclopentene(CPE) using hydrogen peroxide as green oxidant,KCl as cocatalyst and polystyrene-divinylbenzene(PS-DVB) grafted quaternary ammonium phosphor tungsten heterpoly acid salts as tri-phase phase transfer catalysts.Effects of the amount of catalyst and cocatalyst,reaction temperature,reaction time and the molar ratio of CPE to hydrogen peroxide on the product yield were investigated. The suitable reaction conditions with solvent-free were obtained as follows(based on 0.056 mol H2O2):catalyst 1.0 g,cocatalyst 0.025 g,reaction temperature 40℃,reaction time 5h,n(CPE):n(H2O2)=2.1:1.0. Under these conditions,the average yield of CPEO was about 96%. The catalysts can be recovered and even reused for six times without significant decrease of catalytic activity.
2010, 27(12): 1396-1402
doi: 10.3724/SP.J.1095.2010.00127
Abstract:
A new compound of N-(pyrimidin-2-yl)-N'-ethoxylacyl thiourea was synthesized by mixing 2-amino-pyrimidine,potassium thiocyanate and ethyl chloroformate in ethyl acetate,and the structure was characterized by elemental and IR analysis.Single crystals suitable for X-ray measurement were obtained by slow evaporation of dimethylformamide at room temperature.The compound crystallizes in the monoclinic space group P21/n and has a=0.49095(19) nm,b=1.5143(6) nm,c=1.4071(6) nm,β=94.047(8)°,V=1.0435(7) nm3,Z=4,Dc=1.453 g/cm3,μ=0.297 mm-1,F(000)=480,R1=0.0526,wR2=0.1556. There are two intramolecular hydrogen bonds. The synergetic interaction between the electrostatic attraction and hydrogen bondings is responsible for the packing of the compound into three-dimensional network. A crystal unit of the title compound was selected as the initial structure,and it was fully optimized by HF/6-311G,MP2/6-311G and B3LYP/6-311G methods in Gaussian 03 package,the atomic charges,natural bond orbital(NBO),total energy and frontier orbital energy were also discussed,and the thiourea and pyrimidine ring are the active center.
A new compound of N-(pyrimidin-2-yl)-N'-ethoxylacyl thiourea was synthesized by mixing 2-amino-pyrimidine,potassium thiocyanate and ethyl chloroformate in ethyl acetate,and the structure was characterized by elemental and IR analysis.Single crystals suitable for X-ray measurement were obtained by slow evaporation of dimethylformamide at room temperature.The compound crystallizes in the monoclinic space group P21/n and has a=0.49095(19) nm,b=1.5143(6) nm,c=1.4071(6) nm,β=94.047(8)°,V=1.0435(7) nm3,Z=4,Dc=1.453 g/cm3,μ=0.297 mm-1,F(000)=480,R1=0.0526,wR
2010, 27(12): 1403-1408
doi: 10.3724/SP.J.1095.2010.00128
Abstract:
Three novel cuprous complexes of[Cu(L)2](BF4)(a),[LCu(PPh3)2](BF4)(b) and[LCu(POP)](BF4)(c)(L=2-pyridylmethyldiphenylphosphine,POP=bis[2-(diphenylphosphino) phenyl] ether) have been prepared,and characterized by 1H NMR,31P NMR,elemental analysis,and X-ray single-crystal diffraction. X-ray diffraction studies have revealed that the central Cu(Ⅰ) ions of all complexes have a distorted tetrahedral coordination geometry. The complexes show intense π-π* absorption bands in the range of 261~274 nm in deaerated CH2Cl2 solution,while no characteristic metal-ligand charge transfer(MLCT) transition bands appear obviously. In rigid polymethylmethacrylate(PMMA) matrix,these CuⅠ complexes show intense blue emission at 515,476,and 481 nm,with a quantum efficiency of 16.0%,12.9% and 7.0%,respectively. Multilayer organic light-emitting diodes(OLEDs) using poly(N-vinylcarbazole)(PVK) and complex b were fabricated. A current efficiency of 0.36 cd/A and the maximum brightness of 217 cd/m2 have been achieved at current density of 1.0 × 10-3 A/cm2.
Three novel cuprous complexes of[Cu(L)2](BF4)(a),[LCu(PPh3)2](BF4)(b) and[LCu(POP)](BF4)(c)(L=2-pyridylmethyldiphenylphosphine,POP=bis[2-(diphenylphosphino) phenyl] ether) have been prepared,and characterized by 1H NMR,31P NMR,elemental analysis,and X-ray single-crystal diffraction. X-ray diffraction studies have revealed that the central Cu(Ⅰ) ions of all complexes have a distorted tetrahedral coordination geometry. The complexes show intense π-π* absorption bands in the range of 261~274 nm in deaerated CH2Cl2 solution,while no characteristic metal-ligand charge transfer(MLCT) transition bands appear obviously. In rigid polymethylmethacrylate(PMMA) matrix,these CuⅠ complexes show intense blue emission at 515,476,and 481 nm,with a quantum efficiency of 16.0%,12.9% and 7.0%,respectively. Multilayer organic light-emitting diodes(OLEDs) using poly(N-vinylcarbazole)(PVK) and complex b were fabricated. A current efficiency of 0.36 cd/A and the maximum brightness of 217 cd/m2 have been achieved at current density of 1.0 × 10-3 A/cm2.
2010, 27(12): 1409-1412
doi: 10.3724/SP.J.1095.2010.00126
Abstract:
Using the layer-by-layer deposition method,the CdSe-CuTAPPI composite films were obtained on quartz substrate with CdSe nanoparticles and meso-tetra-(4-trimethylaminophenyl) porphyrin copper iodide(CuTAPPI) molecules as assembly units based on electrostatic interactions.The structure,morphology and thickness of the films could well be controlled in a nanoscale.The result of UV-Vis spectra indicated that the consecutive adsorption is uniform and regular,and the nearly equal amount of CuTAPPI and CdSe nanoparticles was assembled into mulilayers in each deposition cycle.The SEM images displayed that the distribution of the nanoparticles in the composite films was uniform,and there was little defects in the films.The influences of aging in the air and irradiation under UV-light on the photoluminescence properties of the CdSe-CuTAPPI composite film were investigated by using fluorescence spectroscopy in detail.It was showed that there existed a stronger interaction between CdSe nanoparticles and CuTAPPI molecules.So the photo-induced electron transfer can be produced from CuTAPPI to CdSe.Furthermore,the photo-stability of CuTAPPI in the composite film was higher.
Using the layer-by-layer deposition method,the CdSe-CuTAPPI composite films were obtained on quartz substrate with CdSe nanoparticles and meso-tetra-(4-trimethylaminophenyl) porphyrin copper iodide(CuTAPPI) molecules as assembly units based on electrostatic interactions.The structure,morphology and thickness of the films could well be controlled in a nanoscale.The result of UV-Vis spectra indicated that the consecutive adsorption is uniform and regular,and the nearly equal amount of CuTAPPI and CdSe nanoparticles was assembled into mulilayers in each deposition cycle.The SEM images displayed that the distribution of the nanoparticles in the composite films was uniform,and there was little defects in the films.The influences of aging in the air and irradiation under UV-light on the photoluminescence properties of the CdSe-CuTAPPI composite film were investigated by using fluorescence spectroscopy in detail.It was showed that there existed a stronger interaction between CdSe nanoparticles and CuTAPPI molecules.So the photo-induced electron transfer can be produced from CuTAPPI to CdSe.Furthermore,the photo-stability of CuTAPPI in the composite film was higher.
2010, 27(12): 1413-1418
doi: 10.3724/SP.J.1095.2010.00038
Abstract:
TiO2-yNx nanoparticles were prepared by in situ doping sol-gel method using urea as the nitrogen source. Their visible-light photocatalytic activity was evaluated by the photocatalytic degradation of methylene blue(MB) in an aqueous solution under visible-light irradiation.The effects of original pH value,nitrogen-doping content and calcination temperature on the as-prepared samples were investigated.The visible-light responsive mechanism of the N-doped sample was studied by means of XRD,XPS,ESR and DRS. The results show that the optimal conditions for the preparation of TiO2-yNx nano-particles are as follows:original pH value 0.52,doping proportion of n(N) to n(Ti) 1:6,and calcination temperature 440℃. The as-prepared sample of single anatase phase with 0.77% N atoms and with average crystal size 19.0 nm exhibits a good visible-light photocatalytic activity. N-doping leads to increasing the surface hydroxyl groups and forming abundant surface oxygen vacancies bounding single-electrons. The O atoms in the TiO2 lattice are substituted by the doped N atoms so that form the N-Ti-O and O-N-Ti bonding structures.N-doping results in a remarkable red-shift of the TiO2 absorption band-edge and significantly increases the absorption of visible-light.The results indicate that N-doping changes the electronic structure of TiO2 and decreases the band-gap.The visible-light response of the N-doped sample is ascribed to a synergetic effect of impurity and defect energy levels that are originated from the substitutional N-doping and the formation of oxygen vacancies accordingly.
TiO2-yNx nanoparticles were prepared by in situ doping sol-gel method using urea as the nitrogen source. Their visible-light photocatalytic activity was evaluated by the photocatalytic degradation of methylene blue(MB) in an aqueous solution under visible-light irradiation.The effects of original pH value,nitrogen-doping content and calcination temperature on the as-prepared samples were investigated.The visible-light responsive mechanism of the N-doped sample was studied by means of XRD,XPS,ESR and DRS. The results show that the optimal conditions for the preparation of TiO2-yNx nano-particles are as follows:original pH value 0.52,doping proportion of n(N) to n(Ti) 1:6,and calcination temperature 440℃. The as-prepared sample of single anatase phase with 0.77% N atoms and with average crystal size 19.0 nm exhibits a good visible-light photocatalytic activity. N-doping leads to increasing the surface hydroxyl groups and forming abundant surface oxygen vacancies bounding single-electrons. The O atoms in the TiO2 lattice are substituted by the doped N atoms so that form the N-Ti-O and O-N-Ti bonding structures.N-doping results in a remarkable red-shift of the TiO2 absorption band-edge and significantly increases the absorption of visible-light.The results indicate that N-doping changes the electronic structure of TiO2 and decreases the band-gap.The visible-light response of the N-doped sample is ascribed to a synergetic effect of impurity and defect energy levels that are originated from the substitutional N-doping and the formation of oxygen vacancies accordingly.
2010, 27(12): 1419-1423
doi: 10.3724/SP.J.1095.2010.00039
Abstract:
Fe2O3,heteropoly salt and Fe/ZrO2 exhibited high catalytic activity toward phenol hydroxylation using H2O2 as oxidant. A rapid hydroxylation of phenol was observed after an induction period in the hydroxylation of phenol catalyzed by Fe2O3;however,a slow hydroxylation of phenol was observed and the induction period disappeared in the same system catalyzed by heteropoly salt or Fe/ZrO2. The results suggest that,first,an induction period in hydroxylation of phenol is related to the formation of active species Fe3+ and Fe2+ from Fe2O3; and second,the slow hydroxylation is related to the surface catalysis reaction on heteropoly salt or Fe/ZrO2,leading to the disappearance of the induction period.
Fe2O3,heteropoly salt and Fe/ZrO2 exhibited high catalytic activity toward phenol hydroxylation using H2O2 as oxidant. A rapid hydroxylation of phenol was observed after an induction period in the hydroxylation of phenol catalyzed by Fe2O3;however,a slow hydroxylation of phenol was observed and the induction period disappeared in the same system catalyzed by heteropoly salt or Fe/ZrO2. The results suggest that,first,an induction period in hydroxylation of phenol is related to the formation of active species Fe3+ and Fe2+ from Fe2O3; and second,the slow hydroxylation is related to the surface catalysis reaction on heteropoly salt or Fe/ZrO2,leading to the disappearance of the induction period.
2010, 27(12): 1424-1429
doi: 10.3724/SP.J.1095.2010.00041
Abstract:
Cobalt/polythiophene/carbon black composite catalysts(Co-PTh/C) were firstly synthesized by an oxidative chemical polymerization and then were tested as a reduction reagent in the gas diffusion electrode of zinc-air cells.The as-prepared catalysts were characterized by means of SEM-EDX and TEM techniques,which showed that they dispersed uniformly and had a size range of 10 to 30 nm.The catalytic activity of the products towards ORR(oxygen reduction reaction) in a 6 mol/L KOH aqueous solution was evaluated by cathodic polarization curves(LSV) and electrochemical impedance spectroscopy(EIS).A current density of 0.152 A/cm2 at-0.20 V(vs.Hg/HgO) could be achieved on the electrode with Co-PTh/C as catalyst,which is superior to 5% Pt/C.Using this electrode as a positive electrode and pure zinc as a negative electrode,a zinc-air cell could be assembled.The cell showed a stable voltage platform of 1.1 V with a constant current density of 0.075 A/cm2 when discharged in a 6.0 mol/L KOH solution.
Cobalt/polythiophene/carbon black composite catalysts(Co-PTh/C) were firstly synthesized by an oxidative chemical polymerization and then were tested as a reduction reagent in the gas diffusion electrode of zinc-air cells.The as-prepared catalysts were characterized by means of SEM-EDX and TEM techniques,which showed that they dispersed uniformly and had a size range of 10 to 30 nm.The catalytic activity of the products towards ORR(oxygen reduction reaction) in a 6 mol/L KOH aqueous solution was evaluated by cathodic polarization curves(LSV) and electrochemical impedance spectroscopy(EIS).A current density of 0.152 A/cm2 at-0.20 V(vs.Hg/HgO) could be achieved on the electrode with Co-PTh/C as catalyst,which is superior to 5% Pt/C.Using this electrode as a positive electrode and pure zinc as a negative electrode,a zinc-air cell could be assembled.The cell showed a stable voltage platform of 1.1 V with a constant current density of 0.075 A/cm2 when discharged in a 6.0 mol/L KOH solution.
2010, 27(12): 1430-1433
doi: 10.3724/SP.J.1095.2010.00096
Abstract:
Ni(OH)2 doped with carbon(C-Ni(OH)2) microsphere was prepared by the hydrothermal method via starting with sodium gluconate and nitrate nickel. The precipitant OH- comes from the hydrolysis of sodium gluconate's carboxylic acid. The as-prepared C-Ni(OH)2 microsphere was adopted as the precursor for fabricating Ni doped with carbon(C-Ni) microsphere by calcined 8 h at 600℃ in N2,and the resulting C-Ni microsphere was further characterized by FE-SEM,XRD,EDS,and BET,verifying the C-Ni microsphere possess considerable large surface area and pore volume of about 276 m2/g and 0.248cm3/g,respectively. Finally,the electrochemical experiment showed that C-Ni microsphere exhibited good electrocatalytic activity toward the oxidation of glucose.
Ni(OH)2 doped with carbon(C-Ni(OH)2) microsphere was prepared by the hydrothermal method via starting with sodium gluconate and nitrate nickel. The precipitant OH- comes from the hydrolysis of sodium gluconate's carboxylic acid. The as-prepared C-Ni(OH)2 microsphere was adopted as the precursor for fabricating Ni doped with carbon(C-Ni) microsphere by calcined 8 h at 600℃ in N2,and the resulting C-Ni microsphere was further characterized by FE-SEM,XRD,EDS,and BET,verifying the C-Ni microsphere possess considerable large surface area and pore volume of about 276 m2/g and 0.248cm3/g,respectively. Finally,the electrochemical experiment showed that C-Ni microsphere exhibited good electrocatalytic activity toward the oxidation of glucose.
2010, 27(12): 1434-1437
doi: 10.3724/SP.J.1095.2010.00116
Abstract:
In this paper,we report a facile approach to obtain different polymorphs of L-glutamic acid(LGA) by crystallization on self-assembled monolayers of L-cysteine under different pH conditions. The β-glutamic acid crystals with plate-like shape were obtained at pH=2.0 and 2.5,while α-glutamic acid crystals were prepared at pH=3.0 and 4.0.The XRD results show that a small amount of β-glutamic acid crystals appear in α-glutamic acid crystals,and they are probably from the secondary nucleation of the β-form.
In this paper,we report a facile approach to obtain different polymorphs of L-glutamic acid(LGA) by crystallization on self-assembled monolayers of L-cysteine under different pH conditions. The β-glutamic acid crystals with plate-like shape were obtained at pH=2.0 and 2.5,while α-glutamic acid crystals were prepared at pH=3.0 and 4.0.The XRD results show that a small amount of β-glutamic acid crystals appear in α-glutamic acid crystals,and they are probably from the secondary nucleation of the β-form.
2010, 27(12): 1438-1443
doi: 10.3724/SP.J.1095.2010.00281
Abstract:
Copper acetate was decomposed by microwave heating to form Cu2O and Cu nanoparticles and Cu/Cu2O core/shell nanostructures. The crystal structures,compositions and morphologies of the products were characterized by powder X-ray diffraction(XRD),transmission electron microscopy(TEM) and scanning electron microscopy(SEM). The diameter of the as-prepared Cu/Cu2O core/shell nanostructures is about 500 nm. Controlled experiments found that polymerization degree of ethylene glycol,reaction time,surfactant or ligand have great effects on the morphology and composition of the products. Lower polymerization degree and longer reaction time facilitate the reduction of copper acetate to form Cu nanoparticles.
Copper acetate was decomposed by microwave heating to form Cu2O and Cu nanoparticles and Cu/Cu2O core/shell nanostructures. The crystal structures,compositions and morphologies of the products were characterized by powder X-ray diffraction(XRD),transmission electron microscopy(TEM) and scanning electron microscopy(SEM). The diameter of the as-prepared Cu/Cu2O core/shell nanostructures is about 500 nm. Controlled experiments found that polymerization degree of ethylene glycol,reaction time,surfactant or ligand have great effects on the morphology and composition of the products. Lower polymerization degree and longer reaction time facilitate the reduction of copper acetate to form Cu nanoparticles.
2010, 27(12): 1444-1450
doi: 10.3724/SP.J.1095.2010.00115
Abstract:
Complexation-ultrafiltration process was investigated for selective separation of Hg(Ⅱ),Cu(Ⅱ) and Cd(Ⅱ) from mixture aqueous solutions.This process included the addition of poly(acrylic acid) sodium salt as a water soluble polymer to selectively bind the metal cations,which was followed by an ultrafiltration operation.Effects of pH and loading ratio(LR) on the selective separation were investigated.It was found that controlling pH=5 was helpful to achieve the selective separation. When LR increased from 0.01 to 2,metal separation coefficients(SHg-Cd and SHg-Cu) increased gradually,and then reached maximum values at LR=2.A concentration experiment was carried out at pH=5 and LR=2.Initial mass concentrations for Hg(Ⅱ),Cu(Ⅱ) and Cd(Ⅱ) were all 30 mg/L.Result showed that,when volume concentration factor(VCF) reached 15,mercury mass concentration of mercury(ρr,Hg),copper(ρr,Cu) and cadmium(ρr,Cd) in the retentate were 435.3 mg/L,42.6 mg/L and 34.2 mg/L,respectively. SHg-Cd、SHg-Cu and SCu-Cd did not change with VCF,and were 229.3,184.3 and 1.2,respectively. This indicated that Hg(Ⅱ) was retained selectively in the retentate by the ultrafiltration operation while nearly all Cu(Ⅱ) and Cd(Ⅱ) passed through the membrane into the permeate.Then,the final concentrated solution was used to study the washing process.With increasing the washing water volume,ρr,Hg remained nearly constant while both ρr,Cu and ρr,Cd decreased rapidly. After doubling the washing water volume,ρr,Cu and ρr,Cd reached 12.54 mg/L and 4.73 mg/L respectively. Further,another concentration experiment was performed at LR=0.033 and pH=5 by using the permeate solutions containing Cu(Ⅱ) and Cd(Ⅱ). At VCF=16,ρr,Cu increased linearly from the beginning of 27.34 mg/L to the end of 430.9 mg/L,whereas ρr,Cd changed only from 27.83 mg/L to 61.5 mg/L. SCu-Cd was 95.8,therefore copper was selectively concentrated.
Complexation-ultrafiltration process was investigated for selective separation of Hg(Ⅱ),Cu(Ⅱ) and Cd(Ⅱ) from mixture aqueous solutions.This process included the addition of poly(acrylic acid) sodium salt as a water soluble polymer to selectively bind the metal cations,which was followed by an ultrafiltration operation.Effects of pH and loading ratio(LR) on the selective separation were investigated.It was found that controlling pH=5 was helpful to achieve the selective separation. When LR increased from 0.01 to 2,metal separation coefficients(SHg-Cd and SHg-Cu) increased gradually,and then reached maximum values at LR=2.A concentration experiment was carried out at pH=5 and LR=2.Initial mass concentrations for Hg(Ⅱ),Cu(Ⅱ) and Cd(Ⅱ) were all 30 mg/L.Result showed that,when volume concentration factor(VCF) reached 15,mercury mass concentration of mercury(ρr,Hg),copper(ρr,Cu) and cadmium(ρr,Cd) in the retentate were 435.3 mg/L,42.6 mg/L and 34.2 mg/L,respectively. SHg-Cd、SHg-Cu and SCu-Cd did not change with VCF,and were 229.3,184.3 and 1.2,respectively. This indicated that Hg(Ⅱ) was retained selectively in the retentate by the ultrafiltration operation while nearly all Cu(Ⅱ) and Cd(Ⅱ) passed through the membrane into the permeate.Then,the final concentrated solution was used to study the washing process.With increasing the washing water volume,ρr,Hg remained nearly constant while both ρr,Cu and ρr,Cd decreased rapidly. After doubling the washing water volume,ρr,Cu and ρr,Cd reached 12.54 mg/L and 4.73 mg/L respectively. Further,another concentration experiment was performed at LR=0.033 and pH=5 by using the permeate solutions containing Cu(Ⅱ) and Cd(Ⅱ). At VCF=16,ρr,Cu increased linearly from the beginning of 27.34 mg/L to the end of 430.9 mg/L,whereas ρr,Cd changed only from 27.83 mg/L to 61.5 mg/L. SCu-Cd was 95.8,therefore copper was selectively concentrated.
2010, 27(12): 1451-1456
doi: 10.3724/SP.J.1095.2010.00109
Abstract:
Interpenetrating polydivinylbenzene/poly(methyl acrylate) polymeric macroporous network(PDVB/PMA IPN) was prepared by sequential suspension polymerization method.By converting PMA into PAA,a hydrophobic-hydrophilic macroporous polydivinylbenzene/poly(acrylic acid) IPN(PDVB/PAA IPN) was achieved.The adsorption thermodynamics and adsorption kinetics of the hydrophobic-hydrophilic IPN were studied.The pore structure,weak acid exchange capacity,water retention capacity and swelling ratio of PDVB/PAA IPN resin were measured.The study focused on the adsorption isotherms of phenylamine at different temperatures.Isosteric adsorption enthalpy,Gibbs free energy and entropy can be calculated according to thermodynamic functions.Infrared spectra results showed that PDVB/PAA IPN resin was successfully synthesized.Compared with the PDVB,PDVB/PMA IPN resin,the BET surface area and pore volume of the PDVB/PAA IPN resin were decreased significantly.The weak acid exchange capacity was 1.91 mmol/g.The water retention capacity was 62.73%.The adsorption of phenylamine was found to be an exothermic process.The experiments of the swelling ratio and the static desorption revealed that the hydrophobic PDVB part in PDVB/PAA IPN resin was responsible for the adsorption of phenylamine through hydrophobic interaction,while the hydrophilic PAA part could adsorb phenylamine by means of hydrogen bondings.The adsorption of phenylamine onto the PDVB/PAA IPN resin reached the equilibrium after 90 min.The adsorption kinetic data of phenylamine fitted the first order rate equation.The intrapartical diffusion of phenylamine was the main rate-controlling step.Adsorption rate was also affected by the film diffusion.The adsorption kinetic data of phenylamine could be described by HSDM model.
Interpenetrating polydivinylbenzene/poly(methyl acrylate) polymeric macroporous network(PDVB/PMA IPN) was prepared by sequential suspension polymerization method.By converting PMA into PAA,a hydrophobic-hydrophilic macroporous polydivinylbenzene/poly(acrylic acid) IPN(PDVB/PAA IPN) was achieved.The adsorption thermodynamics and adsorption kinetics of the hydrophobic-hydrophilic IPN were studied.The pore structure,weak acid exchange capacity,water retention capacity and swelling ratio of PDVB/PAA IPN resin were measured.The study focused on the adsorption isotherms of phenylamine at different temperatures.Isosteric adsorption enthalpy,Gibbs free energy and entropy can be calculated according to thermodynamic functions.Infrared spectra results showed that PDVB/PAA IPN resin was successfully synthesized.Compared with the PDVB,PDVB/PMA IPN resin,the BET surface area and pore volume of the PDVB/PAA IPN resin were decreased significantly.The weak acid exchange capacity was 1.91 mmol/g.The water retention capacity was 62.73%.The adsorption of phenylamine was found to be an exothermic process.The experiments of the swelling ratio and the static desorption revealed that the hydrophobic PDVB part in PDVB/PAA IPN resin was responsible for the adsorption of phenylamine through hydrophobic interaction,while the hydrophilic PAA part could adsorb phenylamine by means of hydrogen bondings.The adsorption of phenylamine onto the PDVB/PAA IPN resin reached the equilibrium after 90 min.The adsorption kinetic data of phenylamine fitted the first order rate equation.The intrapartical diffusion of phenylamine was the main rate-controlling step.Adsorption rate was also affected by the film diffusion.The adsorption kinetic data of phenylamine could be described by HSDM model.
2010, 27(12): 1457-1461
doi: 10.3724/SP.J.1095.2010.00056
Abstract:
SiO2/TiO2 hybrid materials were prepared via a sol-gel process followed with modification by bifunctional reagent of 3-(methoxy-silane-yl) propyl methacrylate(γ-MAPS).A new type of organic-inorganic hybrid capillary monolithic column was prepared in the capillary tube by in-situ polymerization of modified SiO2/TiO2 sol and poly-methyl-propyl-butyl acrylate(BMA).The microstructures of the bed-column cross-section were characterized by scanning electron microscopy(SEM). The column efficiency of 88000 plates per meter was obtained on the basis of evaluating the performance of the as-prepared monolithic column using thiourea as the electroosmotic flow(EOF) marker and investigating the stability and reproducibility of the column as well as the retention behavior of the neutral material on the column.The phosphorpeptide's effective enrichment and separation were realized by the elution test of two kinds of short peptides(phosphoric acid peptide and non-phosphorylated peptides).
SiO2/TiO2 hybrid materials were prepared via a sol-gel process followed with modification by bifunctional reagent of 3-(methoxy-silane-yl) propyl methacrylate(γ-MAPS).A new type of organic-inorganic hybrid capillary monolithic column was prepared in the capillary tube by in-situ polymerization of modified SiO2/TiO2 sol and poly-methyl-propyl-butyl acrylate(BMA).The microstructures of the bed-column cross-section were characterized by scanning electron microscopy(SEM). The column efficiency of 88000 plates per meter was obtained on the basis of evaluating the performance of the as-prepared monolithic column using thiourea as the electroosmotic flow(EOF) marker and investigating the stability and reproducibility of the column as well as the retention behavior of the neutral material on the column.The phosphorpeptide's effective enrichment and separation were realized by the elution test of two kinds of short peptides(phosphoric acid peptide and non-phosphorylated peptides).
2010, 27(12): 1462-1465
doi: 10.3724/SP.J.1095.2010.00099
Abstract:
The enormous quantity impurity of iro (Ⅱ) in the liquids of sulfuric acid oxygen titanium,the intermediate during the production of titanium dioxide,was removed by solvent extraction. Iron(Ⅱ) in the sulfuric acid oxygen titanium liquid was firstly oxidized to iron(Ⅲ) that could be extracted by tri-n-butyl phosphate(TBP) and kerosene mixture system. Various influencing factors on the extraction efficiency of iron(Ⅲ) were investigated,such as the category of oxidant and thinner,the TBP concentration in organic phase,the phase ratio of extraction,the addition of NaCl,the condition of reverse extraction as well as the reuse of the extracting agents.The result showed that a three-time extracting percentage of iron(Ⅲ) could reach 99% when the volume ratio of kerosene to TBP was 4:6,the concentration of NaCl was 4 mol/L and the phase ratio(O/W) was 2:1.The three-time reverse-extract percentage of iron(Ⅲ) reach to 100% when the phase ratio of reverse extraction was 1:1. The extracting percentage of iron(Ⅲ) did not decline significantly even though TBP has been recycled for 5 times.
The enormous quantity impurity of iro (Ⅱ) in the liquids of sulfuric acid oxygen titanium,the intermediate during the production of titanium dioxide,was removed by solvent extraction. Iron(Ⅱ) in the sulfuric acid oxygen titanium liquid was firstly oxidized to iron(Ⅲ) that could be extracted by tri-n-butyl phosphate(TBP) and kerosene mixture system. Various influencing factors on the extraction efficiency of iron(Ⅲ) were investigated,such as the category of oxidant and thinner,the TBP concentration in organic phase,the phase ratio of extraction,the addition of NaCl,the condition of reverse extraction as well as the reuse of the extracting agents.The result showed that a three-time extracting percentage of iron(Ⅲ) could reach 99% when the volume ratio of kerosene to TBP was 4:6,the concentration of NaCl was 4 mol/L and the phase ratio(O/W) was 2:1.The three-time reverse-extract percentage of iron(Ⅲ) reach to 100% when the phase ratio of reverse extraction was 1:1. The extracting percentage of iron(Ⅲ) did not decline significantly even though TBP has been recycled for 5 times.
2010, 27(12): 1466-1469
doi: 10.3724/SP.J.1095.2010.00067
Abstract:
Comamonas testosteroni secretes 3α-HSD/CR when induced by steroid hormones,then it has the characteristics to degrade steroid hormones.This work developed a Enzyme-linked immunosorbent assay(ELISA) method to detect the steroidal hormones in water,food and animal feed.The results show that the content of testosterone and 3α-HSD enzyme expression have a linear relationship.The linear range is within 0.5~600 μg/L.Adopting this method,the study detect the steroidal hormones in water,food and feed.Content of testosterone in Songhua Lake is 34.5 μg/L,which is higher than others.Content of testosterone in the 8 animal feed is more than 2 μg/L.Meat sample test shows that the amount of steroidal hormones is below the detection limit.This result from this method is consistent with that from HPLC.
Comamonas testosteroni secretes 3α-HSD/CR when induced by steroid hormones,then it has the characteristics to degrade steroid hormones.This work developed a Enzyme-linked immunosorbent assay(ELISA) method to detect the steroidal hormones in water,food and animal feed.The results show that the content of testosterone and 3α-HSD enzyme expression have a linear relationship.The linear range is within 0.5~600 μg/L.Adopting this method,the study detect the steroidal hormones in water,food and feed.Content of testosterone in Songhua Lake is 34.5 μg/L,which is higher than others.Content of testosterone in the 8 animal feed is more than 2 μg/L.Meat sample test shows that the amount of steroidal hormones is below the detection limit.This result from this method is consistent with that from HPLC.
2010, 27(12): 1470-1473
doi: 10.3724/SP.J.1095.2010.00107
Abstract:
In hydrochloric acid solution with pH=4.1,Bi(Ⅲ) can react with alizarin red(AR) and cetyltrimethylammonium bromide(CTMAB) to form ternary ion-association complexe particles (the combination proportion was defined as n(Bi(Ⅲ)):n(AR):n(CTMAB)=1:3:3). In this case,the resonance light scattering(RLS) intensities are enhanced greatly. The maximum RLS wavelength locates at 364 nm.The optimal conditions of the reaction,influence factors and the effect of coexisting substances were investigated.In addition,the reaction mechanism of the ternary ion-association complex was discussed. Under the optimal experimental conditions of 2.5 mL 1.0 × 10-4 mol/L alizarim red and 2.0 mL 1.0 × 10-4 mol/L CTMAB,the resonance scattering intensity(△I364 nm) was linearly related to the concentration of Bi(Ⅲ) in the range of 0~0.384 mg/L with a detection limit of 5.898×10-8 g/L. The method can be applied to the determination of Bi(Ⅲ) in water samples. The result was satisfactory and the recoveries were 99.5%~100.2% at the concentrations ranging from 0.552 to 0.831 μg/L,and the relative standard deviation was less than 2.7%. A sensitive,simple and new resonance light scattering method for determination of trace amount of Bi(Ⅲ) in environment was set up using the alizarin red as a spectrum probe.
In hydrochloric acid solution with pH=4.1,Bi(Ⅲ) can react with alizarin red(AR) and cetyltrimethylammonium bromide(CTMAB) to form ternary ion-association complexe particles (the combination proportion was defined as n(Bi(Ⅲ)):n(AR):n(CTMAB)=1:3:3). In this case,the resonance light scattering(RLS) intensities are enhanced greatly. The maximum RLS wavelength locates at 364 nm.The optimal conditions of the reaction,influence factors and the effect of coexisting substances were investigated.In addition,the reaction mechanism of the ternary ion-association complex was discussed. Under the optimal experimental conditions of 2.5 mL 1.0 × 10-4 mol/L alizarim red and 2.0 mL 1.0 × 10-4 mol/L CTMAB,the resonance scattering intensity(△I364 nm) was linearly related to the concentration of Bi(Ⅲ) in the range of 0~0.384 mg/L with a detection limit of 5.898×10-8 g/L. The method can be applied to the determination of Bi(Ⅲ) in water samples. The result was satisfactory and the recoveries were 99.5%~100.2% at the concentrations ranging from 0.552 to 0.831 μg/L,and the relative standard deviation was less than 2.7%. A sensitive,simple and new resonance light scattering method for determination of trace amount of Bi(Ⅲ) in environment was set up using the alizarin red as a spectrum probe.
2010, 27(12): 1474-1477
doi: 10.3724/SP.J.1095.2010.00125
Abstract:
A resonance light scattering detection method of ascorbic acid is reported based on the formation of silver nanoparticles(NPs).Ascorbic acid(vitamin C,VC) could reduce Ag(NH3)2+ to form the silver nanoparticles,resulting in strong plasmon resonance light scattering(PRLS) signals characterized at 544 nm,which could be measured using a common spectrofluorometer.It is found that the PRLS intensities were proportional to the ascorbic acid concentrations in the range of 0.2~7.0 μmol/L with R2=0.9988 and detection limit(3σ/k) of 8.1 × 10-9 mol/L. The presence of a physically adsorbed layer of the product of the redox reaction on the surface of colloidal silver could prevent irreversible aggregation of silver NPs. The conditions of the reaction and the interference of the common ions are investigated. For the determination of ascorbic acid in VC tablets and beverage samples.The recovery was within the range of 94.5%~97.0%. Results suggested that the method possessed easy of implementation,high sensitivity,and better recovery,and so on.
A resonance light scattering detection method of ascorbic acid is reported based on the formation of silver nanoparticles(NPs).Ascorbic acid(vitamin C,VC) could reduce Ag(NH3)2+ to form the silver nanoparticles,resulting in strong plasmon resonance light scattering(PRLS) signals characterized at 544 nm,which could be measured using a common spectrofluorometer.It is found that the PRLS intensities were proportional to the ascorbic acid concentrations in the range of 0.2~7.0 μmol/L with R2=0.9988 and detection limit(3σ/k) of 8.1 × 10-9 mol/L. The presence of a physically adsorbed layer of the product of the redox reaction on the surface of colloidal silver could prevent irreversible aggregation of silver NPs. The conditions of the reaction and the interference of the common ions are investigated. For the determination of ascorbic acid in VC tablets and beverage samples.The recovery was within the range of 94.5%~97.0%. Results suggested that the method possessed easy of implementation,high sensitivity,and better recovery,and so on.
2010, 27(12): 1478-1480
doi: 10.3724/SP.J.1095.2010.00059
Abstract:
The synthetic method of a new aromatic diacid,9,9-bis[4-(4-carboxyphenoxy) phenyl]xanthene(4) was developed from the reaction of 9,9-bis(4-hydroxyphenyl) xanthene(1) with 4-methyl-1-iodobenzene(2) by means of the Ullmann coupling and oxidation reaction successively. The treatment of compound 1 with compound 2 in DMF in the presence of cuprous iodide/tetrabutylammonium bromide/potassium phosphate at reflux temperature for 24 h afforded 9,9-bis[4-(4-methylphenoxy) phenyl]xanthene(3) in 95% yield.The compound 3 was then oxidized to the corresponding aromatic,9,9-bis[4-(4-carboxyphenoxy) phenyl]xanthene(4) in 84% yield directly using oxygen in the presence of a catalytic amount of N-bromosuccinimde(NBS) under photoirradiation. The new diacid 4 was obtained in an overall yield of about 79.8%(based on compound 1). The structure of the target compound was characterized by 1H NMR,13C NMR,IR and elemental analysis. The present method has the advantage of convenient availability of starting materials,mild reaction conditions,convenient manipulation and good yield.
The synthetic method of a new aromatic diacid,9,9-bis[4-(4-carboxyphenoxy) phenyl]xanthene(4) was developed from the reaction of 9,9-bis(4-hydroxyphenyl) xanthene(1) with 4-methyl-1-iodobenzene(2) by means of the Ullmann coupling and oxidation reaction successively. The treatment of compound 1 with compound 2 in DMF in the presence of cuprous iodide/tetrabutylammonium bromide/potassium phosphate at reflux temperature for 24 h afforded 9,9-bis[4-(4-methylphenoxy) phenyl]xanthene(3) in 95% yield.The compound 3 was then oxidized to the corresponding aromatic,9,9-bis[4-(4-carboxyphenoxy) phenyl]xanthene(4) in 84% yield directly using oxygen in the presence of a catalytic amount of N-bromosuccinimde(NBS) under photoirradiation. The new diacid 4 was obtained in an overall yield of about 79.8%(based on compound 1). The structure of the target compound was characterized by 1H NMR,13C NMR,IR and elemental analysis. The present method has the advantage of convenient availability of starting materials,mild reaction conditions,convenient manipulation and good yield.
2010, 27(12): 1481-1482
doi: 10.3724/SP.J.1095.2010.00092
Abstract:
The effects of non-rare earths impurities,such as Fe,Si,Al on the formation of emulsion phase were studied in the extraction of yttrium with naphthenic acid,and Si was found to be most significant one.Different solutions for removing the feed solutions were provided and an oxidation absorption precipitation method was proven to be the most effective approach,which can remove the emulsion phase in the extraction of rare earths.
The effects of non-rare earths impurities,such as Fe,Si,Al on the formation of emulsion phase were studied in the extraction of yttrium with naphthenic acid,and Si was found to be most significant one.Different solutions for removing the feed solutions were provided and an oxidation absorption precipitation method was proven to be the most effective approach,which can remove the emulsion phase in the extraction of rare earths.
2010, 27(12): 1483-1485
doi: 10.3724/SP.J.1095.2010.00052
Abstract:
Supercritical CO2 fluid(SFE-CO2) extraction technique was used to extract the rare ginsenosides in processed ginseng,and extracting productions were analyzed by HPLC/ESI-MSn. The optimal extraction conditions were estimated as:the extraction pressure was 35 MPa,the extraction temperature was at 50℃,and the concentration of alcohol as entrainer was 70%. The experimental result showed that the extracting efficiency of SFE-CO2 technique is similar with that of transonic extraction. The extracting method using SFE-CO2 technique is in favor of ambient.
Supercritical CO2 fluid(SFE-CO2) extraction technique was used to extract the rare ginsenosides in processed ginseng,and extracting productions were analyzed by HPLC/ESI-MSn. The optimal extraction conditions were estimated as:the extraction pressure was 35 MPa,the extraction temperature was at 50℃,and the concentration of alcohol as entrainer was 70%. The experimental result showed that the extracting efficiency of SFE-CO2 technique is similar with that of transonic extraction. The extracting method using SFE-CO2 technique is in favor of ambient.
2010, 27(12): 1486-1488
doi: 10.3724/SP.J.1095.2010.00061
Abstract:
Further separation of the ethyl acetate extractive of Senecio scandens Buch.-Ham.,four flavonoids and two phenolic acids were isolated by chromatography and identified by physico-chemical properties,NMR and MS,as isoquercitrin(Ⅰ),hyperin(Ⅱ),chlorogenic acid(Ⅲ),caffeic acid(Ⅳ),quercetin(Ⅴ) and isorhamnetin(Ⅵ). Compound Ⅰ was isolated from plant of Senecio genus for the first time,and compounds Ⅱ~Ⅵ were isolated from the plant for the first time.
Further separation of the ethyl acetate extractive of Senecio scandens Buch.-Ham.,four flavonoids and two phenolic acids were isolated by chromatography and identified by physico-chemical properties,NMR and MS,as isoquercitrin(Ⅰ),hyperin(Ⅱ),chlorogenic acid(Ⅲ),caffeic acid(Ⅳ),quercetin(Ⅴ) and isorhamnetin(Ⅵ). Compound Ⅰ was isolated from plant of Senecio genus for the first time,and compounds Ⅱ~Ⅵ were isolated from the plant for the first time.
